СПОСОБ ПОЛУЧЕНИЯ (НИТРОКСИМЕТИЛ)ФЕНИЛ ЭФИРОВ ПРОИЗВОДНЫХ САЛИЦИЛОВОЙ КИСЛОТЫ

Изобретение относится к способу получения (нитроксиметил)фенил эфиров производных салициловой кислоты формулы (I) где R1 означает OCOR3 группу, где R3 означает метил, этил или линейный или разветвленный С3-С5 алкил;R2 означает водород. Способ включает следующие стадии: а) реакция галогенида производного салициловой кислоты с гидроксибензиловым спиртом в присутствии основания в органическом растворителе; b) нитрование полученного продукта в безводных условиях в инертном органическом растворителе, имеющего точку кипения ниже, чем 200°С при атмосферном давлении, смесью азотной кислоты с отличной неорганической кислотой, или органической кислотой, или ангидридом одной или двух органических кислот; с) выделение конечного продукта. Технический результат – удешевление процесса, уменьшение побочных реакций, увеличение выхода продукта. 5 з.п. ф-лы, 1 табл.

УСТРОЙСТВО ДЛЯ НИТРОВАНИЯ СПИРТОВ

Устройство для нитрования спиртов, отличающееся тем, что оно состоит из двух вертикально расположенных секций, первая секция состоит из вращающейся камеры смешения, выполненной в виде колеса центробежного насоса, между верхним и нижним дисками которого расположены перегородки в виде спиралей, а патрубки подачи смеси спиртов и кислоты введены в полость колеса на меньшем диаметре, причем сливные концы патрубков в полости колеса расположены на минимальном расстоянии друг от друга, вторая секция состоит из камеры смешения, выполненной в виде конического корпуса, снабженного в верхней части кольцевой полостью, в которой концентрично установлена камера смешения первой секции, причем кольцевая полость снабжена отражательным диском, внутренний диаметр которого составляет 0,5÷0,7 диаметра колеса.

НИТРОЭФИРЫ, ОБЛАДАЮЩИЕ ПРОТИВОВОСПАЛИТЕЛЬНОЙ И/ИЛИ АНАЛЬГЕТИЧЕСКОЙ АКТИВНОСТЬЮ, СПОСОБЫ ИХ ПОЛУЧЕНИЯ, ФАРМАЦЕВТИЧЕСКИЕ КОМПОЗИЦИИ

Нитроэфиры формулы M-CO-Y-(C)nAB-ONO2, где А и В - водород или метил; М выбирают из соединений формулы I-IV R - остаток формулы V-VII Y - О, NH, NR1; R1 - алкил, n = 1-6, пригодны для лечения тяжелых состояний, требующих одновременно применения противовоспалительных и анальгетических лекарственных препаратов, или ревматических заболеваний общего характера. 5 с. и 12 з.п. ф-лы, 2 ил., 5 табл.

НИТРАТОР ДЛЯ ПОЛУЧЕНИЯ ЖИДКИХ НИТРОЭФИРОВ

FIELD: chemistry. SUBSTANCE: invention relates to production of nitric acid esters used in production of ballistic powder, industrial explosives and liquid monofuels, particularly to a nitrate for producing liquid nitroesters. Proposed nitrator comprises enclosed in a housing with a cover and rotating on a vertical shaft an open-top plate with a disc fixed thereon by radial partitions and equipped with sides bent upwards, forming a toroid-shaped cavity, and introduced into torus space a mixing tube, end of which is directed towards rotation of plate and is arranged with minimum possible gap relative to surface of plate, tube for supplying nitro mixture into centre of plate and tube for supplying alcohol with arrangement thereof from intake end of mixing tube at a distance, corresponding to turning angle of plate about its axis by 100-180°. Nitrator is equipped with a baffle plate in form of vertically arranged curved plate with unclosed cylindrical surface, in cross section representing an arc segment with a central angle of 180°. Beginning of plate is located in zone of intake end of mixing tube with following continuation in direction of rotation of plate. Upper end plate is attached to outer surface of cover of housing, and lower end is bent at an angle of 25-35° and inserted into torus space of plate. Radius of arc of baffle is smaller than radius of edge of bent sides of plate. EFFECT: nitrator increases safety of nitration process due to creation of conditions to prevent drops of reaction liquid falling onto surface of housing of nitrator and preventing decomposition thereof without using cooling while maintaining dimensions of nitrator and dwell time therein. 1 cl, 1 dwg РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2 603 773 C1 (51) МПК C07C 201/02 (2006.01) B01J 19/00 (2006.01) B01F 5/00 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ОПИСАНИЕ (21)(22) Заявка: ИЗОБРЕТЕНИЯ К ПАТЕНТУ 2015143512/04, 12.10.2015 (24) Дата начала отсчета срока ...

СПОСОБ ПОЛУЧЕНИЯ НИТРОЭФИРОВ ОДНОАТОМНЫХ СПИРТОВ

Изобретение относится к способу получения нитроэфиров одноатомных спиртов, которые находят применение в качестве эффективных цетанповышающих присадок к дизельным топливам. Предлагается способ получения сложных эфиров одноатомных спиртов путем их обработки серно-азотной кислотной смесью в присутствии карбамида, сепарацию кислого нитроэфира и последующую его промывку, в котором в качестве одноатомного спирта используют 2-этилгексанол и/или изоамиловый спирт, серно-азотную кислотную смесь состава, мас.%: НNО- 18,0-21,0 НSO- 62,0-65,0 вода - остальное до 100, которую готовят из 99,8%-ной НNО, 93,4%-ной НSOи отработанной кислоты, получаемой в процессе нитровании, обработку серно-азотной кислотной смесью проводят при температуре не выше 25-30°С в течение 25-30 минут, а промывку кислого нитроэфира осуществляют вначале промывной водой при соотношении продукт:промывная вода 1:0,5, а затем 2%-ным раствором гидроокиси натрия при соотношении 1:0,3. Способ получения нитроэфиров одноатомных спиртов позволяет ...

СПОСОБ ПОЛУЧЕНИЯ МОНОНИТРАТА 1,4-БУТАНДИОЛА

... 1. Способ получения 4-нитрооксибутан-1-ола, включающий: ! стадию а) взаимодействие избытка 1,4-бутандиол с кислотой формулы R-C(O)OH, где R - линейная или разветвленная (С3-С5)-алкильная цепь, в присутствии кислого катализатора и в алифатическом неполярном растворителе, с последующим селективным отделением моноэфира 1,4-бутандиола формулы (I) ! ! где R как указано выше, от реакционной смеси; ! стадию b) нитрование RC(O)O-(CH2)4-ОН смесью концентрированной H2SO4 и концентрированной HNO3 или смесью азотной кислоты и уксусной кислоты или уксусного ангидрида с последующим выделением моноэфира 4-нитрооксибутан-1-ола формулы (II) ! ! где R как указано выше; ! стадию с) селективный гидролиз алкилкарбоксильного фрагмента соединения (II) неорганическим основанием в однослойной системе с последующей очисткой 4-нитрооксибутан-1-ола формулы (III) ! ! характеризующийся тем, что стадию нитрования осуществляют, используя моноэфир 1,4-бутандиола формулы (I), содержащий 1,4-бутандиол в количестве менее ...

НИТРАТЫ СПИРТОВ, СОДЕРЖАЩИЕ АМИДНУЮ, ДИНИТРОМЕТИЛЕНОВУЮ И НИТРАМИННУЮ ГРУППЫ, СПОСОБ ИХ ПОЛУЧЕНИЯ; 3-(АЦИЛАМИНОДИНИТРОАЛКИЛ)-ТЕТРАГИДРО-1,3-ОКСАЗОЛЫ И - ОКСАЗИНЫ, СПОСОБ ИХ ПОЛУЧЕНИЯ

... 1. Нитраты спиртов, содержащие амидную, динитрометиленовую и нитраминную группы, общей формулы (I) R'C(O)N(R")(CH2)nC(NO2)2CH2N(NO2)(CH2)mONO2, где R'=-CH3, R''=-СН2ОН, n=1, m=2 (1) R'=-CH3, R''=-H, n=1, m=2 (2) R'=-CH3, R''=-CH2OH, n=2, m=2 (3) R'=-CH3, R''=-H, n=2, m=2 (4) R'=-CH3, R''=-CH2OH, n=1, m=3 (5) R'=-CH3, R''=-H, n=1, m=3 (6) R''=-CH2OH, n=1, m=2 (7) R''=-CH2OH, n=1, m=3 (8) 2. Способ получения нитратов спиртов общей формулы (I) R'C(O)N(R")(CH2)nC(NO2)2CH2N(NO2 )(CH2)mONO2, где R'=-CH3, R''=-СН2ОН, n=1, m=2 (1) R'=-CH3, R''=-H, n=1, m=2 (2) R'=-CH3, R''=-CH2OH, n=2, m=2 (3) R'=-CH3, R''=-H, n=2, m=2 (4) R'=-CH3, R''=-CH2OH, n=1, m=3 (5) R'=-CH3, R''=-H, n=1, m=3 (6) R"=-CH2OH, n=1, m=2 (7) R"=-CH2OH, n=1, m=3 (8) путем нитрования, отличающийся тем, что действуют нитрующим средством на 3-(ациламинодинитроалкил)-тетрагидро-1,3-оксазолы и -оксазины при 0-60° с последующим разбавлением реакционной массы водой и выделением целевого продукта. 3. Способ по п.2, отличающийся тем, что ...

СПОСОБ ПОЛУЧЕНИЯ 2-ЭТИЛГЕКСИЛНИТРАТА

БЕЗОПАСНЫЙ СПОСОБ ПОЛУЧЕНИЯ АЛИФАТИЧЕСКИХ ПОЛИНИТРАТОВ СПИРТОВ В ПРОМЫШЛЕННЫХ УСЛОВИЯХ

Изобретение относится к способу получения полинитратов многоатомных алифатических спиртов. Способ заключается в нитровании соответствующих многоатомных алифатических спиртов серно-азотными смесями. Нитрование проводят в емкостном реакторе периодического действия, снабженном рубашкой, змеевиком, донным сифоном и нижним аварийным сливом, в который последовательно вводят при перемешивании растворы концентрированной серной и азотной кислот с общим содержанием воды не более 10-15% и смесь индифферентных хлорорганических растворителей. Первый из растворителей представляет собой сравнительно низкокипящий индифферентный хлорорганический растворитель (т.кип. не более 60°С), а второй - сравнительно высококипящий индифферентный хлорорганический растворитель (т.кип. 60-120°С). Затем дозируют нитруемое соединение со скоростью, обеспечивающей температурный режим не выше 16°С. Предлагаемый способ является безопасным и позволяет с высоким выходом получать полинитраты многоатомных алифатических спиртов.

Способ получения нитратов органических соединений

Process of and apparatus for uninterruptedly washing nitroglycerine, nitroglycol and like esters

... 284,702. Schmid, A., and Meissner, J., (Assignees of Dynamit-Akt.-Ges. vorm. A. Nobel & Co.). Feb. 5, 1927, [Convention date]. Nitroglycerine, nitroglycol &c. are washed free from acid by supplying the liquid through a pipe 4, and a washing liquid, such as soda solution, through a pipe 5, to the base of a columnar vessel 1 divided by horizontal perforated partitions 2. Compressed air is supplied through a pipe 6 and carries the mixture of liquid upwards through the screens 2 to an outlet 7 leading to a separator. The Specification as open to inspection under Sect. 91 (3) (a) describes also that in place of using compressed air, a vertical rotary shaft having stirring arms in the compartments between the screens 2 may be used. This subject-matter does not appear in the Specification as accepted.

Process for preparing mononitrochlorobenzene

Improvements in the manufacture of explosives

In the nitration of organic compounds involving heating or cooling of one or more of the reagents, temperature-controlling media are employed for the whole of such heating or cooling which are in indirect contact with the reagents and are inert to them or react to form innocuous products. Explosion or fire through leakage from the heating or cooling system is thereby avoided. The media may consist of substances present in the reagents. Thus in nitrating glycerine or glycol, the cooling medium is nitric or sulphuric acid or a mixture thereof having a water content substantially that of the nitrating acid. The cooling medium may then be used to feed the nitrator. Inert saturated aliphatic hydrocarbons or halogenated hydrocarbons, or solutions of nitrates and/or sulphates can also be used. These are circulated between the cooling coils, jackets, or the like of the nitrator and a refrigerating machine. Alternatively, an inert gas such as carbon dioxide or air may be employed. For heating the ...

NEW ALKALOID DERIVATIVE AND THIS CONTAINING PHARMACEUTICAL COMPOSITION

PROCEDURE FOR THE PRODUCTION OF NITRIC ACID ESTERS OF UNIVALENT ALCOHOLS

4-NITROXYBUTYLESTER OF NAPROXEN

Process for preparing nitrooxyderivatives of naproxen

NITRATED HIGH ENERGY MATERIALS

PROCESS FOR PRODUCTION OF ALKYL NITRITE

PROCESS AND REACTION VESSEL FOR PRODUCTION OF ALKYL NITRITE A process and reaction vessel for producing alkyl nitrite is disclosed, the process comprising (a) contacting nitric oxide, lower alcohol and oxygen in a reaction zone such that alkyl nitrite is formed, said reaction zone comprising a reactor section and a rectification section, (b) supplying a liquid scrubbing agent to an upper portion of the rectification section, (c) withdrawing a gaseous alkyl nitrite product stream from the upper portion of the rectification section, and (d) withdrawing a liquid stream from a lower portion of the reactor section. The reactor section provides intimate vapor-liquid contact sufficient to enhance the conversion of nitric oxide to alkyl nitrite and the rectification section provides sufficient vapor residence time to enhance conversion of oxygen, as well as sufficient rectification capabilities to reduce the amounts of water and nitric acid in the gaseous alkyl nitrite product stream.

NITRATION OF ORGANIC COMPOUNDS

PREPARATION OF NITRONITRATES

PREPARATION OF NITRITE ESTERS

METHOD AND DEVICE FOR REMOVING CONTAMINANTS ARISING DURING THE PRODUCTION OF ALIPHATIC NITRATE ESTERS

The invention relates to a method and to a device for removing contaminants arising during the production of aliphatic or alicyclic nitric acid esters, in particular for removing contaminants from nitrated crude nitric acid esters, which nitrated crude nitric acid esters arise during the nitration of monovalent or multivalent aliphatic or alicyclic alcohols capable of nitration, after the separation of the final nitrating acid, and to a production system for nitrating monovalent or multivalent aliphatic alcohols capable of nitration with subsequent purification of the nitrated nitric acid esters.

NITRIC ESTERS HAVING ANTI-INFLAMMATORY AND/OR ANALGESIC ACTIVITY AND PROCESS FOR THEIR PREPARATION

The present invention refers to nitric esters of derivatives of propionic acid, I(p-chlorobenzoyl)-5-methoxy-2-methyl-3-indolylacetic acid, 5-benzoyl-1,2-dihydro-3H-pyrrolo¢1,2-a!pyrrole-1-carboxylic acid, 6-methoxy-2-naphthylactic acid, having general formula (IA), their pharmaceutical use and the process for their preparation.

Verfahren zur Herstellung heisser Gase mit Hilfe eines Heizöls

Verfahren zur Herstellung von Isopropylnitrat

Verfahren zur Reinigung von Salpetersäureestern

Verfahren zur Herstellung aliphatischer Nitrate.

Verfahren zur Herstellung von Isopropylnitrat.

Séparateur centrifuge pour la séparation de liquides

Procédé de fabrication de composés organiques nitrés.

Verfahren zur Herstellung von Alkylnitraten

Verfahren zur Herstellung von Salpetersäureestern aus aliphatischen Alkoholen

Verfahren zur Herstellung von Salpetersäureestern mehrwertiger Alkohole

Verfahren zur Veresterung mehrwertiger Alkanole mit Salpetersäure

Verfahren zur Herstellung von aliphatischen Nitraten

METHOD AND INSTALLATION FOR DEGRADATION OF NITROGLYCERIN IN THE NITRATION PROCESS WASTE ACIDS.

METHOD FOR SYNTHESIS OF CHEMICAL COMPOUNDS FROM CARBON DIOXIDE

METHOD AND DEVICE FOR REMOVING CONTAMINANTS ARISING DURING THE PRODUCTION OF ALIPHATIC NITRATE ESTERS

Method of using nano oxides to assist in preparing cetane number improver

Formation of nitrate esters in microreactors and millireactors using a continuous product extraction in a turbulent flow regime

Process for the manufacture of nicorandil

Process for the Preparation of Pentaerythritol Tetranitrate Free from Acid, and Explosive Compositions

A method for producing organic nitrated compounds

NUCLEOPHILIC PROCESS OF SUBSTITUTION

Cette invention concerne un procédé de substitution nucléophile d'une fonction hydroxyle d'un alcool par un groupe nucléophile (Nu) autre qu'un atome de fluor, comprenant les étapes de : a) mise en présence de l'alcool avec le nucléophile, puis addition de SF4 ou d'un trifluorure d'aminosoufre, ce qui conduit à la réaction de substitution nucléophile attendue; b) hydrolyse du mélange réactionnel; et c) séparation du produit final obtenu.

NEW DERIVATIVES NITERS ANALGESICS, ANTI-INFLAMMATORY DRUGS AND ANTI-THROMBOTIQUES, THEIR METHOD OF PREPARATION, THEIR APPLICATION LIKE DRUGS

L'invention a pour objet les produits de formule (I): (CF DESSIN DANS BOPI) dans laquelle Ar représente un radical monocyclique ou bicyclique aromatique comportant de 5 à 10 atomes de carbone et éventuellement 1 ou 2 hétéroatomes choisis parmi les atomes d'azote, d'oxygène ou de soufre, ce radical étant lui-même substitué ou non substitué. R1 représente un atome d'hydrogène ou un radical méthyle ou éthyle, n est compris entre 0 et 8, m est compris entre 0 et 8, la somme n + m est comprise entre 0 et 8, p est égal à 0 ou 1, et A représente un radical bivalent dérivé d'un hydrocarbure cyclique saturé comprenant de 3 à 8 atomes de carbone, éventuellement substitué, étant entendu que lorsque m = 0 l'hydrocarbure cyclique saturé ne comprend pas 5 à 7 atomes de carbone et étant entendu que A n'est pas attaché aux groupes (CF DESSIN DANS BOPI) par le même atome de carbone de leur procédé de préparation et les intermédiaires de ce procédé, leur application comme médicaments et les compositions ...

Manufacture of aliphatic nitrates

NITRATE ESTER PREPARATION

processo para preparar ácido 4-nitro-óxi-metil-benzoico

ANALGESIC, ANTI-INFLAMMATORY AND ANTI-THROMBOSIS ESTERS OF NITRATED CYCLOALIPHATIC ALCOHOLS

The invention concerns products of formula (I) in which Ar represents an aromatic monocyclic or bicyclic radical comprising 5 to 10 carbon atoms and optionally 1 or 2 heteroatoms selected among the atoms of nitrogen, oxygen or sulphur, said radical being itself substituted or not; R1 represents a hydrogen atom or a methyl or ethyl radical, n ranges from 0 to 8, m ranges from 0 to 8, the sum n + m ranges from 0 to 8, p is equal to 0 or 1, and A represents a bivalent radical derived from a saturated cyclic hydrocarbon containing 3 to 8 carbon atoms, optionally substituted, being understood that when m = 0 the saturated cyclic hydrocarbon does not contain 5 to 7 carbon atoms and that A is not linked to the groups (a) and (CH2)m-O-No2 by the same carbon atom. The invention also concerns the method for preparing them and the intermediate products of this method, their application as medicine and the pharmaceutical compositions containing them.

NEW PROCESS

The present invention relates to a new process for the preparation of the (S)-naproxen 4-nitrooxybutyl ester and to new intermediates obtained and used therein. The invention further relates to the use of the new intermediates for the manufacturing of pharmaceutically active compounds such as (S)-naproxen 4-nitrooxybutyl ester.The invention also relates to the use of (S )-naproxen 4-nitrooxybutyl ester prepared according to the process of the present invention for the manufacturing of a medicament for the treatment of pain.

PROCESS FOR THE PREPARATION OF (S)- NAPROXEN 4-NITROOXYBUTYL ESTER

The present invention relates to a new process for the preparation of the (S)-naproxen 4-nitrooxybutyl ester and to new intermediates obtained and used therein. The invention further relates to the use of the new intermediates for the manufacturing of pharmaceutically active compounds such as (S)-naproxen 4-nitrooxybutyl ester. The invention also relates to the use of (S)-naproxen 4-nitrooxybutyl ester prepared according to the process of the present invention for the manufacturing of a medicament for the treatment of pain.

MICROBIAL SYNTHESIS OF D-1,2,4-BUTANETRIOL

Improved enzyme systems, recombinant cells, and processes employing the same to produce biosynthetic D-1,2,4-butanetriol; D-1,2,4-butanetriol prepared thereby and derivatives thereof; D-1,2,4-butanetriol trinitrate prepared therefrom; and enzymes and genes useful in the enzyme systems and recombinant cells.

Process for the preparation of naproxene nitroxyalkylesters

A process for obtaining nitroxyalkylesters of the 2-(S)-(6-methoxy-2-naphthyl)-propanoic acid having an enantiomeric excess higher than or equal to 95%, preferably higher than or equal to 98%, characterized in that an halide of the 2-(S)-(6-methoxy-2-naphthyl)-propanoic acid of formula A-Hal, wherein A is the acid acyl residue, is reacted in an inert organic solvent with an aliphatic nitroxyalkanol HO-Y-ONO2, wherein Y is a C2-C20 alkylene or a cycloalkylene from 3 to 8 carbon atoms, or an alkylene as defined containing a cycloalkylene as defined, in the presence of an inorganic base.

A NOVEL ALKALOID DERIVATIVE AND A PHARMACEUTICAL COMPOSITION CONTAINING THE SAME

The present invention is to provide a novel colchicine derivative represented by the formula (I) with halogen or nitric ester group, or pharmaceutically acceptable salts thereof, pharmaceutical compositions containing the same as effective components and having anticancer, anti-proliferous and immunosuppressive functions, and methods for preparing the colchicine derivatives: ...

ТОПЛИВНАЯ КОМПОЗИЦИЯ ДЛЯ ДИЗЕЛЬНЫХ ДВИГАТЕЛЕЙ

Изобретение описывает топливную композицию для дизельных двигателей, характеризующуюся тем, что в качестве присадки к топливу используется смесь 10-25 мас.% смеси алкилнитратов спиртов С-С, 10-25 мас.% смеси простых диалкиловых эфиров на основе спиртов С-Си до 100 мас.% дизельного топлива или любого углеводородного растворителя, причем в качестве исходных спиртов С-Сдля получениясмеси алкилнитратов и смеси простых диалкиловых эфировиспользуют фракцию спиртов C-C, полученных методом жидкофазного окисления фракции н-алканов C-Cводным раствором пероксида водорода в среде метанола на гетерогенном катализаторе ДП-2, и последующего гидрирования реакционной массы на жестком ячеистом катализаторе Pd/AlO. Предлагается также дизельное топливо, содержащее данную присадку в количестве 0,01-0,5 мас.%. Композиция позволяет увеличить цетановое число дизельных топлив на 4-6 единиц и снизить температуру застывания дизельных топлив на 10-15°С. 2 н.п. ф-лы, 2 табл.

СПОСОБ СИНТЕЗА НИТРОКСИМЕТИЛФЕНИЛОВЫХ ЭФИРОВ АСПИРИНА И ЕГО ПРОИЗВОДНЫХ

Изобретение описывает способ синтеза нитроксиметилфениловых эфиров аспирина и его производных. Описывается способ получения (нитроксиметил)фениловых эфиров аспирина и его производных формулы R-COOH с типами радикалов, имеющих следующую формулу: где R1 означает группу OCOR3; где R3 означает метил, этил или алкил С3-С5, линейный или разветвленный; R2 означает водород; nI означает 0; причем вышеупомянутый способ синтеза включает следующие стадии: (1) реакцию между галогенидом R-С(O)-Х1А), где X1 означает Cl, Br, и R означает радикал как определено выше, с изомером гидроксибензальдегида, в присутствии основания, с образованием (карбонил)фенилового эфира (I); (2) восстановление альдегидной группы (карбонил)фенилового эфира с образованием (гидроксиметил)фенилового эфира; (3) реакцию между (гидроксиметил)фениловым эфиром формулы (II) с: a) SOX2, причем Х означает галоген, выбранный между Cl и Br, или b) с тозилхлоридом или мезилхлоридом; (4) реакцию между сложным эфиром, полученным на предыдущей ...

СПОСОБ ПОЛУЧЕНИЯ ЦЕТАНОПОВЫШАЮЩИХ ПРИСАДОК К ДИЗЕЛЬНОМУ ТОПЛИВУ

Изобретение относится к способу получения цетаноповышающих присадок к дизельному топливу, включающему нитрование вторичных спиртов, где в качестве спиртов используют фракцию вторичных спиртов C-C, полученных методом жидкофазного окисления фракции н-алканов C-Cводным раствором пероксида водорода в среде метанола на гетерогенном катализаторе ДП-2, и последующему гидрированию реакционной массы на жестком ячеистом катализаторе P1/AO, нитрование проводят 5-10- кратным мольным избытком азотной кислоты концентрации 50-80% в присутствии 1-5% масс. от массы азотной кислоты гетерогенного суперкислого катализатора на основе сульфатрованного оксида циркония - ZrO/SO /γ-AlOв интервале температур от 0º до 10ºС. Для предотвращения окисления фракции спиртов C-Cазотной кислотой процесс проводят в пристутсвии карбамида в количестве 0,5-5%. Технический результат заключается в сокращении затрат на сырье, уменьшение количества сточных вод, уменьшение количества стадий процесса. При добавлении 0,5% масс. получаемой ...

СПОСОБ ПОЛУЧЕНИЯ 1-НИТРОКСИАДАМАНТАНА

Изобретение относится к области фармацевтической химии, а именно к способу получения 1-нитроксиадамантана, промежуточного продукта в синтезе 1-адамантанкарбоновой кислоты, принципиального промежуточного продукта в синтезе противовирусного препарата ремантадина. Согласно заявляемому способу адамантан добавляют к 10÷15%-ному раствору нитрата аммония в 98%-ной азотной кислоте, взятой в количестве 4,5÷5,6 массовых частей на 1 часть адамантана при температуре 3÷5°С и затем выдерживают 1,5 часа при 22÷25°С, выливают на лед и отделяют продукт реакции. Выход 1-нитроксиадамантана согласно предлагаемому способу 90-91%.

Способ получения цетаноповышающей присадки н-бутилнитрат

Изобретение относится к области органической химии, конкретно к способу получения цетаноповышающей присадки, представляющей собой н-бутилнитрат, путем нитрования спирта смесью серной и азотной кислот. Способ заключается в том, что кислотную смесь состава, мас.%: H2SO4 - 45-60, HNO3 - 10-25, вода - остальное до 100, перемешивают и при температуре реакционной смеси около 15°С в течение 1-1,5 ч дозируют н-бутанол, после чего выдерживают при реакционной температуре в течение 10-20 мин. После этого нижний слой нитрующей смеси сливают и охлаждают, разбавляя 50-60 мас.% воды, и далее направляют на регенерацию серную кислоту, которую используют повторно после восстановления, а верхний слой продукта нитрования охлаждают и промывают 40 мас.% воды при температуре 20-40°С, после чего подают в сепаратор. В сепараторе верхний слой продукта отделяют от промывной воды, содержащей отмытые кислоты, и подают на промывку 45 мас.% водным раствором гидрокарбоната натрия с общей концентрацией гидрокарбоната ...

СПОСОБ ПОЛУЧЕНИЯ 4-НИТРООКСИМЕТИЛБЕНЗОЙНОЙ КИСЛОТЫ

... 1. Способ получения 4-нитрооксиметилбензойной кислоты формулы (I)включающий реакцию 4-хлорметилбензойной кислоты (III)с нитратом серебра в присутствии кислоты в качестве катализатора в ацетонитриле при температуре кипения с обратным холодильником, охлаждение, добавление первого полярного непротонного растворителя, отделение образовавшихся солей серебра посредством фильтрации и промывание отфильтрованных солей серебра вторым полярным непротонным растворителем с образованием фильтрата, осаждение соединения (I) водой из фильтрата и сушку соединения (I).2. Способ по п.1, в котором кислота выбрана из группы кислот, включающей бензолсульфоновую, бромистоводородную, хлористоводородную, хлоруксусную, хлорсульфоновую, этансульфоновую, фосфорную, метансульфоновую, азотную, п-хлорбензолсульфоновую, п-толуолсульфоновую, серную, трихлоруксусную, трихлорметансульфоновую, трифторуксусную и трифторметансульфоновую и их смесей.3. Способ по п.2, в котором кислота представляет собой серную кислоту.4. Способ ...

СПОСОБ ПОЛУЧЕНИЯ ЦИКЛОГЕКСИЛНИТРАТА

Изобретение относится к технологии органических соединений, а именно к области производства эфиров азотной кислоты. Описывается способ получения циклогексилнитрата, включающий нитрование циклогексанола смесью уксусного ангидрида и азотной кислоты, разбавление реакционной массы водой, отделение органического слоя и его промывку водой и раствором соды, при этом при нитровании смесью уксусного ангидрида и азотной кислоты с мольным соотношением компонентов 1:1 берут 1,80-1,84 в.ч. такой смеси на 1 в.ч. циклогексанола, выдерживают реакционную массу при 18-20°С в течение 60 минут, затем разбавляют водой, взятой в количестве 0,48-0,55 в.ч. на 1 в.ч. реакционной массы, отделяют слой циклогексилнитрата и промывают любым из известных способов, а содержащуюся в отработанной жидкости азотную кислоту нейтрализуют гидроокисью или карбонатом натрия, взятыми к ней в стехиометрическом соотношении с некоторым избытком, после чего отработанную жидкость перегоняют, отбирая первую фракцию, температура кипения ...

СПОСОБ ПОЛУЧЕНИЯ НИТРООКСИПРОИЗВОДНЫХ НАПРОКСЕНА

ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß (19) RU (51) ÌÏÊ 7 (11) 2005 104 419 (13) A C 07 C 201/08, 203/04 ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÇÀßÂÊÀ ÍÀ ÈÇÎÁÐÅÒÅÍÈÅ (21), (22) Çà âêà: 2005104419/04, 06.08.2003 (71) Çà âèòåëü(è): ÍÈÊÎÊÑ Ñ.À. (FR) (30) Ïðèîðèòåò: 29.08.2002 IT MI2002A001861 (43) Äàòà ïóáëèêàöèè çà âêè: 20.11.2005 Áþë. ¹ 32 (86) Çà âêà PCT: EP 03/08698 (06.08.2003) (74) Ïàòåíòíûé ïîâåðåííûé: Êóðûøåâ Âëàäèìèð Âàñèëüåâè÷ Àäðåñ äë ïåðåïèñêè: 121087, Ìîñêâà, à/ 33, Â.Â. Êóðûøåâó Ôîðìóëà èçîáðåòåíè 1. Ñïîñîá ïîëó÷åíè ñîåäèíåíè îáùåé ôîðìóëû (À) A ãäå R îçíà÷àåò R U 2 0 0 5 1 0 4 4 1 9 A (54) ÑÏÎÑÎÁ ÏÎËÓ×ÅÍÈß ÍÈÒÐÎÎÊÑÈÏÐÎÈÇÂÎÄÍÛÕ ÍÀÏÐÎÊÑÅÍÀ â êîòîðîì R' îçíà÷àåò àòîì âîäîðîäà èëè Br; R1-R12 âë þòñ îäèíàêîâûìè èëè ðàçëè÷íûìè è íåçàâèñèìî îçíà÷àþò âîäîðîä, ëèíåéíûé èëè ðàçâåòâëåííûé Ñ1-Ñ6àëêèë, íåîá çàòåëüíî çàìåùåííûé àðèëîì; m, n, î, q, r è s êàæäûé íåçàâèñèìî îçíà÷àåò öåëîå ÷èñëî îò 0 äî 6, è ð îçíà÷àåò 0 Ñòðàíèöà: 1 RU 2 0 0 5 1 0 4 4 1 9 (87) Ïóáëèêàöè PCT: WO 2004/020384 (11.03.2004) R U (85) Äàòà ïåðåâîäà çà âêè PCT íà íàöèîíàëüíóþ ôàçó: 29.03.2005 (72) Àâòîð(û): ÄÅËÜ ÑÎËÄÀÒÎ Ïüåðî (IT), ÑÀÍÒÓÑ Äæèàíêàðëî (IT), ÁÅÍÅÄÈÍÈ Ôðàí÷åñêà (IT) èëè 1, è Õ îçíà÷àåò Î, S, SO, SO2, NR13 èëè PR13, â êîòîðîì R13 îçíà÷àåò âîäîðîä, C1-Ñ6àëêèë, èëè Õ âûáðàí èç ãðóïïû, âêëþ÷àþùåé: öèêëîàëêèëåí ñ 5-7 àòîìàìè óãëåðîäà â öèêëîàëêèëåíîâîì êîëüöå, ïðè ýòîì êîëüöî íåîá çàòåëüíî çàìåùåíî áîêîâûìè öåï ìè Ò, ãäå Ò îçíà÷àåò ëèíåéíûé èëè ðàçâåòâëåííûé àëêèë ñ 1-10 àòîìàìè óãëåðîäà; àðèëåí, íåîá çàòåëüíî çàìåùåííûé îäíèì èëè áîëåå àòîìîâ ãàëîãåíà, ëèíåéíûìè èëè ðàçâåòâëåííûìè àëêèëüíûìè ãðóïïàìè, ñîäåðæàùèìè îò 1 äî 4 àòîìîâ óãëåðîäà, èëè ëèíåéíûì èëè ðàçâåòâëåííûì C1-Ñ3ïåðôòîðàëêèëîì; 5- èëè 6-÷ëåííîå íàñûùåííîå, íåíàñûùåííîå èëè àðîìàòè÷åñêîå ãåòåðîöèêëè÷åñêîå êîëüöî, âûáðàííîå èç Ñòðàíèöà: 2 2 0 0 5 1 0 4 4 1 9 R U A ãäå R1-R2 è m, è, î, ð, q, r, s âë þòñ òàêèìè êàê îïðåäåëåíû âûøå, è Y âûáðàí èç àòîìà ãàëîãåíà, -BF4, -SbF6, FSO3-, RASO3-, â êîòîðîì ...

Способ получения производных N-(бета-фенилвинил)-лактамов или амидов кислот

4-Nitroxybutylester von Naproxen

NITRATED POLYBUTADIENE

... 299,384. Schmid, A., and Meissner, J., (Assignees of Dynamit-Akt.-Ges. vorm. A. Nobel & Co.). Oct. 25, 1927, [Convention date]. Addition to 284,701. Nitroglyerine ; nitroglycol, &c.-In separating nitroglycerine nitroglycol and similar explosives from residual acid used in their manufacture, as described in the parent Specification by passing the liquid through narrow spaces between parallel inclined partitions 2 in a vessel 1, the liquid supplied from an inlet 6 is distributed by being passed through a series of partitions 11 having perforations which are larger in the first partition and which are out of line with each other. Similar perforated partitions are placed in the outlet compartment 13. Cooling coils may be placed between the partitions 11, or parallel cooling pipes with small intermediate spaces may replace the partitions 11.

Manufacture of organic nitrates applicable in the explosives industry

Diethylene glycol is nitrated with an acid mixture comprising by weight, 3-12 per cent of water, 30-60 per cent of nitric acid and 35-60 per cent of sulphuric acid, whilst well agitating the mixture and keeping it cool. A number of examples are given in which the proportion of nitric acid varies between 44,57 and 51,06 per cent, of sulphuric acid between 49,52 and 41,6 per cent, and of water, between 5,91 and 7,34 per cent. During the nitration, the diethylene glycol is allowed to run in a fine stream or streams into the acid mixture cooled down to 10 DEG C., an allowance of from 5 to 10 per cent excess nitric acid over that theoretically required being made. The diethylene glycol dinitrate is readily applied in the explosives industry, either alone, or in admixture with trinitroglycerine or ethylene glycol dinitrate. In admixture with either of the above explosives, a solvent is obtained which dissolves nitrocellulose of 11 to 12 per cent nitrogen content in the cold.

Improvements in the manufacture of alkyl nitrates from alkylenes

C2-4 2-alkyl nitrates are prepared by first absorbing an appropriate alkylene in sulphuric acid in known manner to form a product consisting of at least one alkyl ester of sulphuric acid wherein the ester group is in the 2-position and then continuously reacting the resulting sulphuric ester product with nitric acid at a temperature sufficient to continuously remove the 2-alkyl nitrate formed in the reaction, by introducing said sulphuric ester product continuously into a bulk of hot aqueous nitric acid containing a stabiliser consisting of a compound capable of destroying any nitrous acid formed in the reaction medium and, if desired, also containing sulphuric acid, to which nitric acid is being continuously fed, while the resulting 2-alkyl nitrate is being continuously removed by distillation along with dilute nitric acid. The stabiliser is preferably urea or urea in conjunction with ammonium nitrate. The examples describe the preparation of ethyl, isopropyl and 2-butyl nitrates.

Process for the nitration of organic compounds

Organic compounds which form solid nitration products are continuously nitrated by mixing the starting material with nitric acid, sulphuric acid and a solvent for the nitration product, pumping the resulting liquid reaction mass through a heat exchanger for effecting the reaction, withdrawing the reaction mass from the heat exchanger, withdrawing a lesser portion of said reaction mass and pumping it to a separator for separating the solution of the nitration product from the waste acid, recirculating the residual reaction mass through the heat exchanger and introducing further reaction mass into the circulating stream to maintain the volume substantially constant. The process may be effected in the apparatus of Specification 919,717. An exemplified process nitrates 2,4-din tromethylaniline using dichloroethane as solvent to produce tetryl. Other specified starting compounds are benzene, substituted benzenes, naphthalene, substituted naphthalenes, alkyl benzenes, substituted polyalkyl benzenes ...

MORE SALZETERSAÜREESTER WITH ENTZÜNDUNGSHEMMENDER AND/OR SCHMERZLINDERNDER EFFECT AND PROCEDURE FOR THEIR PRODUCTION

WATER DISTANCE WITH A PROCEDURE FOR CONTINUOUS NITRATING OF A NITRATE-CASH AROMATIC CONNECTION.

NITRATION USING NO2 ) H2O2

Method for nucleophilic substitution

Apparatus and method for continuous production of polyethylene glycol dinitrate

Disclosed is an apparatus for producing polyethylene glycol dinitrate. The apparatus includes providing continuously an acid composition and a glycol composition to a reaction apparatus; reacting the acid composition and the glycol composition in the reaction apparatus in a continuous manner to generate a reaction composition; using an alkaline composition to at least partially neutralize the reaction composition to cause at least a portion of the polyethylene glycol dinitrate to deposit from a solution of the reaction composition; and extracting the deposit of polyethylene glycol dinitrate.

PROCESS FOR THE PREPARATION OF SESQUITERPENES

PREPARATION OF NITRITE ESTERS

PREPARATION OF NITRITE ESTERS A novel process for the vapor phase process for making aliphatic nitrites from aliphatic alcohols by reaction of a nitrogen oxide composition with alcohol. S P E C I F I C A T I O N ...

PROCESS FOR THE PREPARATION OF A NITRIC OXIDE DONATING PROSTAGLANDIN ANALOGUE

The present invention relates to a process for preparing the hexanoic acid, 6-(nitrooxy)-, (1S,2E)-3-[(1R,2R,3S,5R)-2-[(2Z)-7-(ethylamino)-7-oxo-2-hepten-1-yl]- 3,5-dihydroxycyclopentyl]-1-(2-phenylethyl)-2-propen-1-yl ester of formula (I). In accordance with the present invention, the compound (I) can be efficiently prepared with high purity by coupling bimatoprost in a boronate protected form with 6-(nitrooxy)hexanoyl chloride and removing the boronate protecting group. The 6-(nitrooxy)hexanoyl chloride intermediate is prepared by ring-opening reaction of 2-caprolactone and subsequent nitration of the 6-hydroxyhexanoic acid potassium salt with a mixture of HNO3 and H2SO4 in dichloromethane.

PROCESS FOR THE PREPARATION OF SESQUITERPENES

PROCESS FOR THE PRODUCTION OF CHEMICAL COMPOUNDS FROM CARBON DIOXIDE

Process for the production of a chemical compound from a carbon dioxide starting material, comprising the steps of a) providing a feed stream consisting mainly of carbon dioxide; b) electrolysing in an electrolysis stage the carbon dioxide in the feed stream to a first gas stream containing carbon monoxide and a second gas stream containing oxygen, wherein the molar ratio between carbon monoxide and oxygen is about 1:0.5 in an electrolysis stage; c) adjusting the composition of the first gas stream or the second gas stream or both gas streams to include carbon dioxide, either by operating at less than full conversion of CO2 or by sweeping one or both gas streams with a gas containing CO2 or by at some stage between the electrolysis cell and the oxidative carbonylation reactor diluting one or both gas streams with a gas containing CO2; all while maintaining an overall molar ratio of carbon monoxide to oxygen of about 1:0.5; and d) introducing the first and second process stream into a reaction ...

СПОСОБ ПОЛУЧЕНИЯ ХИМИЧЕСКИХ СОЕДИНЕНИЙ ИЗ ДИОКСИДА УГЛЕРОДА

Способ получения химического соединения из исходного материала, содержащего диоксид углерода, включающий следующие этапы: а) получение потока исходного материала, состоящего, главным образом, из диоксида углерода; b) электролиз на этапе электролиза диоксида углерода в потоке поступающего материала с получением первого газового потока, содержащего монооксид углерода, и второго газового потока, содержащего кислород, причем молярное отношение монооксида углерода к кислороду на этапе электролиза составляет приблизительно 1:0,5; с) регулирование композиции таким образом, чтобы первый газовый поток или второй газовый поток или оба газовых потока включали диоксид углерода, либо путем осуществления неполной конверсии CO2, либо путем продувки одного или обоих газовых потоков газом, содержащим CO2, либо на каком-либо этапе между электролизером и реактором окислительного карбонилирования путем разбавления одного или обоих газовых потоков газом, содержащим CO2, при этом поддерживая общее молярное отношение ...

METHOD AND DEVICE FOR REMOVING CONTAMINANTS ARISING DURING THE PRODUCTION OF ALIPHATIC NITRATE ESTERS

СПОСОБ ПОЛУЧЕНИЯ ОРГАНИЧЕСКИХ НИТРАТОВ

В заявке описан способ получения органических нитратов, содержащих по меньшей мере одну нитрилоксигруппу и по меньшей мере одну гидроксигруппу, где по меньшей мере одна гидроксигруппа может существовать в форме этерифицированного гидроксильного остатка, который этерифицирован кислотой, не являющейся азотной кислотой.

METHOD AND APPARATUS FOR REMOVING POLLUTING IMPURITIES, EMERGING IN THE PROCESS OF PRODUCTION OF THE COMPLEX ALIPHATIC OF NITROGEN-ACID ESTERS

Acrylate-terminated polyglycidyl ether nitrate, preparation method and application

The invention discloses acrylate-terminated polyglycidyl ether nitrate as well as a preparation method and application thereof. The structural formula of the disclosed compound is shown as (I). The acrylate-terminated polyglycidyl ether nitrate (APGN) provided by the invention has terminal group double bonds, and can be rapidly cured under ultraviolet light; the acrylate-terminated poly (glycidyl nitrate) (APGN) is an energetic binder, and compared with a halogen-terminated double-bond energetic binder in the prior art, the binder disclosed by the invention does not contain halogen elements, and is clean in combustion and non-corrosive in fuel gas.

NEW DERIVATIVES NITERS ANALGESICS, ANTI-INFLAMMATORY DRUGS AND ANTI-THROMBOTIQUES, THEIR METHOD OF PREPARATION, THEIR APPLICATION LIKE DRUGS

Nitration continues organic compounds, and for example of aromatic hydrocarbons

PROCESS FOR THE PREPARATION OF ALPHA,OMEGA-ALKANEDIOL MONONITRATE

The invention relates to a safe and efficient process for the hydrolysis of α,ω-C3-10alkanediol mononitrate monoacylates. The process is safer to operators and allows to obtain advantageous yields on industrial scale.

NITRATION OF AROMATIC COMPOUNDS

The present invention provides a process for nitrating aromatic compounds without the need for a solid catalyst and/or any organic solvents and/or any other additives. A typical process includes combining or admixing a nitric acid and an anhydride compound under conditions sufficient to produce a reactive intermediate. The aromatic compound to be nitrated is then added to this reactive intermediate to produce a nitroaromatic compound. The nitroaromatic compound can be substituted with one or more, typically, one to three, and often one or two nitrate (-NO2) groups.

METHOD AND DEVICE FOR REMOVING CONTAMINANTS ARISING DURING THE PRODUCTION OF ALIPHATIC NITRATE ESTERS

A process for the production of high energy material

A process for the production of a high energy nitrate ester involves reacting, in an inert organic solvent, a heterocyclic compound, selected from oxiranes, oxetanes, N-substituted aziridines and N-substituted azetidines, with either N2O4 or N2O5, and when the compound is reacted with N2O4, oxidising the O- or N-nitrate substituents or substituent in the product to O- or N-nitrate substituent or substituents. The remaining ring carbon atoms on the heterocyclic compound may be substituted or unsubstituted. Preferred substituent groups for the C and/or N ring atoms on the compound include alkyl, cyanoalkyl, haloalkyl, nitroalkyl, and substituted aryl. Several novel nitrate ester are also provided, including nitrated derivatives of polybutadiene, in which between 1% and 25% of the carbon atoms in the polymer are substituted by vicinal nitrate ester (-ONO2) groups.

SIMULTANEOUS NITRATION

СПОСОБ ПОЛУЧЕНИЯ ЖИДКИХ НИТРОЭФИРОВ И УСТАНОВКА ДЛЯ ЕГО ОСУЩЕСТВЛЕНИЯ

Изобретение относится к области производства эфиров азотной кислоты, используемых при получении баллиститных порохов, промышленных взрывчатых веществ и жидких унитарных топлив. Описывается способ получения жидких нитроэфиров путем нитрования спирта в нитраторе с малым реакционным объемом, охлаждения реакционной смеси в проточном холодильнике, сепарации нитроэмульсии и промывки нитроэфира, при этом нитрование осуществляют в две ступени с полным выводом отработанной кислоты из процесса с промежуточным охлаждением нитромассы после первой ступени, причем в нитратор первой ступени подают 50-60%, а в нитратор второй ступени 50-40% от требуемого количества нитруемого спирта, при этом массовое соотношение нитросмеси и спирта выбирают исключающим достижение температуры разложения нитроэфиров. Также описывается установка для получения жидких нитроэфиров. Технический результат - расширение эксплуатационных возможностей путем снижения производительности в соответствии с существующей потребностью и ...

СПОСОБ ПОЛУЧЕНИЯ НИТРОКСИАЛКИЛОВЫХ ЭФИРОВ НАПРОКСЕНА

Изобретение относится к новому способу получения нитроксиалкиловых эфиров напроксена. Описывается способ получения нитроксиалкиловых эфиров 2-(S)-(6-метокси-2-нафтил)-пропановой кислоты с энантиомерным избытком, превышающим или равным 97%, предпочтительно превышающим или равным 98%, при этом галогенангидрид 2-(S)-(6-метокси-2-нафтил)-пропановой кислоты формулы A-Hal, где A представляет собой ацильный остаток указанной кислоты, подвергают взаимодействию в инертном органическом растворителе с алифатическим нитроксиалкиловым спиртом HO-Y-ONO2, где Y является линейным или необязательно разветвленным С2-С5 алкиленом, в присутствии неорганического основания и получают соответствующий нитроксиалкиловый эфир 2-(S)-(6-метокси-2-нафтил)-пропановой кислоты формулы A-O-Y-ONO2, где А и Y такие, как определено выше. Также описывается 4-нитроксибутиловый эфир 2-(S)-(6-метокси-2-нафтил)-пропановой кислоты с энантиомерным избытком (S) формы в пределах от 97% до 98%, предпочтительно свыше 98%. Технический ...

СПОСОБ ПОЛУЧЕНИЯ 1,1,2,2-ТЕТРАКИС-(НИТРОКСИМЕТИЛ)-1,2-ДИНИТРОЭТАНА

Способ получения 1,1,2,2-тетракис-(нитроксиметил)-1,2-динитроэтана из 5,5'-бис-(2,2-диметил-5-нитро-1,3-Диоксана) путем постадийного гидролиза и нитрования продукта гидролиза, отличающийся тем, что гидролиз и нитрование продукта проводят в одну стадию путем обработки его концентрированной азотной кислотой.

Способ получения н-бутилнитрата

Изобретение относится к химической и топливной промышленности, к области производства нитроэфиров, конкретно к способу получения н-бутилнитрата, применяемому в качестве цетаноповышающей добавки к дизельному топливу. Способ характеризуется тем, что предварительно в н-бутанол вводят карбамид в количестве 0,5-1 мас.% от его массы, нитрование ведут в тарельчатом нитраторе, при этом нитрующая смесь содержит 60-65 мас.% серной кислоты, 15-20 мас.% азотной кислоты, остальное - вода, отношение массы нитрующей смеси к массе н-бутанола составляет 15-20. После сепарации смеси промывку н-бутилнитрата осуществляют последовательно водой с массовым соотношением вода : н-бутилнитрат, равным (1,0-1,5):1, 2-3%-ным раствором кальцинированной соды с массовым соотношением раствор : н-бутилнитрат, равным (1,0-1,5):1, а затем снова водой с массовым соотношением вода : н-бутилнитрат, равным (1,0-1,5):1. Техническим результатом изобретения является повышение устойчивости и стабильности процесса нитрования н-бутанола ...

Способ получения нитроэфиров

FIELD: chemistry.SUBSTANCE: invention relates to chemistry of organic nitro compounds, specifically to a method of producing nitroesters of general formula R(ONO), where n = 1–3, R is a mono-, di- or trivalent hydrocarbon radical C-C, or a bivalent radical containing one or more oxygen atoms in the carbon chain, by reacting corresponding alcohols with a nitrogen-containing (V) nitrating agent in a flow-type reactor at room temperature in liquefied 1,1,1,2-tetrafluoroethane (TFE) medium with subsequent treatment of the reaction mass with aqueous sodium hydroxide solution and the process is carried out in molar ratio of initial alcohol: nitrogen oxide (V): sodium hydroxide 1:1–3.6:1–3.4 with residence time of the reaction mass in reactor from 4 to 100 s and pressure from 0.8 to 1.0 MPa.EFFECT: technical result achieved when implementing the disclosed method of producing nitroesters is to increase specific efficiency of the process.1 cl, 1 dwg, 17 ex РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2 689 406 C1 (51) МПК C07C 201/02 (2006.01) C07C 201/08 (2006.01) C07C 203/04 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ (52) СПК C07C 201/02 (2019.02); C07C 201/08 (2019.02); C07C 203/04 (2019.02) (21)(22) Заявка: 2019101405, 18.01.2019 (24) Дата начала отсчета срока действия патента: Дата регистрации: 28.05.2019 (45) Опубликовано: 28.05.2019 Бюл. № 16 трехвалентный углеводородный радикал С3-C8, либо двухвалентный радикал, содержащий в углеродной цепи один или несколько атомов кислорода, путем взаимодействия соответствующих спиртов с нитрующим агентом - оксидом азота (V) в реакторе проточного типа при комнатной температуре в среде сжиженного R U 2 6 8 9 4 0 6 (54) Способ получения нитроэфиров (57) Реферат: Изобретение относится к области химии органических нитросоединений, а именно, к способу получения нитроэфиров общей формулой R(ONO2)n, где n=1-3, R - одно-, двух- или Стр.: 1 (56) Список документов, цитированных в отчете о ...

4-Nitroxybutylester von Naproxen

Epoxidation of glycerol and derivatives therefrom

A method producing a surfactant from glycerol by converting glycerol, in a first step, to glycidol, polymerizing glycidol to an aliphatic alcohol and finally substituting a hydroxyl group with a substitute anion.

Process for the preparation of latanoprostene bunod and intermediate thereof and compositions comprising the same

Processes for preparing latanoprostene bunod and an intermediate prepared from the process. Also latanoprostene bunod compositions having high-purity latanoprostene bunod.

SAFE METHOD FOR PRODUCING ALKYL NITRATE

The present invention provides a method for producing alkyl nitrate. The centrifugal extraction equipment acts as the esterification separator; a mixed acid solution containing sulfuric acid and nitric acid enters from the heavy phase inlet of the centrifugal extraction equipment; alkyl alcohol enters from the light phase inlet of the centrifugal extraction equipment; the feeding molar ratio of alkyl alcohol and nitric acid equals to 1:1.0-3.0; esterification reaction occurs with the mixed acid and alkyl alcohol at a temperature of 10˜60° C. under the rotating speed of 800-2000 r/min; under the action of centrifugal force, the generated coarse ester as a light phase and the spent acid as a heavy phase are separated; coarse ester as a light phase is discharged through the light-phase outlet of the centrifugal extractor; the spent acid as a heavy phase is discharged through the heavy-phase outlet of the centrifugal extractor; after alkali washing and water washing conventionally, coarse ester is dehydrated for drying and purified, then the refining products of alkyl nitrate is obtained. In the method of the present invention, esterification reaction, the separation of reaction products and the spent acid are finished in the same reactor simultaneously, which reduces the contact time of reaction products with the spent acid greatly, avoids the side reaction effectively, and ensures the safety of esterification process. 1. A method for producing alkyl nitrate , wherein , comprising the steps of:1) The centrifugal extraction equipment acts as the esterification separator; a mixed acid solution containing sulfuric acid and nitric acid enters from the heavy phase inlet of the centrifugal extraction equipment; alkyl alcohol enters from the light phase inlet of the centrifugal extraction equipment; the feeding molar ratio of alkyl alcohol and nitric acid equals to 1:1.0-3.0; esterification reaction occurs with the mixed acid and alkyl alcohol at a temperature of 10˜60° C. ...

Utilizing Nitrate Salts in Order to Produce Explosives

Mass production of industrial explosives with one-tenth of the cost of the current production method—Nitric acid 98% removal of the chemical reaction producing explosive materials—Increasing the production safety—Producing ammonium sulfate, a chemical fertilizer, as a byproduct—Supporting the production of different explosives such as TNT, nitroglycerine and etc.—decreasing the acid concentration in the product.

METHOD AND APPARATUS FOR PRODUCING ALKYL NITRITE

A method for producing an alkyl nitrite by bringing an aqueous solution containing nitric acid and an alkanol into contact with a gas including nitrogen monoxide and thereby producing an alkyl nitrite, in which the reaction temperature is 60° C. to 100° C., is provided. 1. A method for producing an alkyl nitrite , the method comprising:bringing an aqueous solution containing nitric acid and an alkanol into contact with a gas including nitrogen monoxide and thereby producing an alkyl nitrite, wherein a reaction temperature is 60° C. to 100° C.2. The method for producing an alkyl nitrite according to claim 1 , wherein a concentration of the alkanol is 50% by weight to 80% by weight with respect to the total amount of the aqueous solution.3. The method for producing an alkyl nitrite according to claim 1 , wherein a concentration of the alkanol is 60% by weight or more with respect to the total amount of the aqueous solution.4. The method for producing an alkyl nitrite according to claim 1 , wherein a concentration of nitric acid in a reaction liquid obtainable by bringing the aqueous solution into contact with the gas is decreased to 1% by weight or less.5. The method for producing an alkyl nitrite according to claim 1 , wherein the alkanol includes methanol.6. The method for producing an alkyl nitrite according to claim 1 , wherein a concentration of nitric acid in the aqueous solution is 1% by weight to 20% by weight with respect to the total amount of the aqueous solution.7. The method for producing an alkyl nitrite according to claim 1 , the method comprising:a first reaction step of producing the alkyl nitrite at a reaction temperature of 60° C. to 80° C.; anda second reaction step of producing the alkyl nitrite at a reaction temperature of 80° C. to 100° C.8. The method for producing an alkyl nitrite according to claim 7 , wherein a superficial gas velocity in the first reaction step is 20 mm/second to 100 mm/second claim 7 , and a superficial gas velocity in the ...

CONTINUOUS SYNTHESIS OF ISOOCTYL NITRATE IN A FLOW REACTOR

A process for synthesizing isooctyl nitrate in a continuous flow reactor comprises flowing a H2SO4—HNO3 mixture within a flow reactor, flowing isooctyl alcohol into said flow reactor so as to mix the isooctyl alcohol with the H2SO4—HNO3 mixture and produce a reaction mixture stream flowing in said reactor, maintaining the reaction mixture stream flowing in said flow reactor at a reaction temperature within in the range −10° to 35° C. inclusive, and wherein the residence time of the reaction mixture stream in the flow reactor is greater than or equal to 5 seconds and less than or equal to 40 seconds, and wherein the H2SO4 of the H2SO4—HNO3 mixture is H2SO4 having a concentration of in the range of 85 to 95% inclusive, more desirably 88 to 92% inclusive, most desirably of 90%. 1. A process for synthesizing isooctyl nitrate in a continuous flow reactor with 99% or greater conversion and 99% or greater yield , the process comprising:flowing a H2SO4—HNO3 mixture within a flow reactor;flowing isooctyl alcohol into said flow reactor so as to mix the isooctyl alcohol with the H2SO4—HNO3 mixture and produce a reaction mixture stream flowing in said reactor;maintaining the reaction mixture stream flowing in said flow reactor at a reaction temperature within in the range −10° to 35° C. inclusive,wherein the residence time of the reaction mixture stream in the flow reactor is in the range of 5 to 40 seconds, inclusive, and wherein the H2SO4 of the H2SO4—HNO3 mixture is H2SO4 having a strength within the range of 85% to 95% inclusive.2. The process according to wherein the H2SO4 of the H2SO4—HNO3 mixture is H2SO4 having a strength within the range of 88% to 92% inclusive.3. The process according to wherein the H2SO4 of the H2SO4—HNO3 mixture is 90% H2SO4.4. The process according to wherein the step of flowing a H2SO4—HNO3 mixture within a flow reactor comprises flowing a H2SO4 stream into a first inlet of the flow reactor and flowing a HNO3 stream into a second inlet of the flow ...

Highly z-selective and enantioselective ring opening/cross metathesis catalyzed by a resolved stereogenic-at-ru complex

This invention relates generally to enantiomerically enriched C—H activated ruthenium olefin metathesis catalyst compounds which are stereogenic at ruthenium, to the preparation of such compounds, and the use of such catalysts in the metathesis of olefins and olefin compounds, more particularly, in the use of such catalysts in enantio- and Z-selective olefin metathesis reactions. The invention has utility in the fields of catalysis, organic synthesis, polymer chemistry, and industrial and fine chemicals chemistry.

METHOD FOR PREPARING NITRATE ESTER

A method for preparing a nitrate ester is provided. The method includes providing a first solution including a compound (which has at least one hydroxyl group) and a carboxylic acid having 2-5 carbon atoms; providing a second solution including nitric acid, acetic anhydride, and acetic acid; and transferring the first solution and the second solution to a microreactor, obtaining a nitrate ester after a residence time. In particular, the ratio of the weight of nitric acid to the total volume of the acetic anhydride and acetic acid is 1:1 to 1:3.5. The ratio of the molar amount of nitric acid to the hydroxyl group equivalent of the compound is from 1:1 to 15:1. 1. A method for preparing nitrate ester , comprising:providing a first solution, wherein the first solution consists of a compound and a carboxylic acid having 2-5 carbon atoms, wherein the compound has at least one hydroxyl group;providing a second solution, wherein the second solution consists of nitric acid, acetic anhydride and acetic acid, wherein the ratio of the weight of nitric acid to the total volume of the acetic anhydride and acetic acid is 1:1 to 1:3.5; andtransferring the first solution and the second solution to a microreactor to form a mixture, obtaining a nitrate ester after a residence time, wherein the ratio of the molar amount of nitric acid in the mixture to the hydroxyl group equivalent of the compound in the mixture is from 1:1 to 15:1.2. The method for preparing nitrate ester as claimed in claim 1 , wherein nitric acid has a concentration not less than 98%.3. The method for preparing nitrate ester as claimed in claim 1 , wherein the carboxylic acid having 2-5 carbon atoms is acetic acid claim 1 , propionic acid claim 1 , butyric acid claim 1 , or pentanoic acid.4. The method for preparing nitrate ester as claimed in claim 1 , wherein the residence time is from 30s to 200s.5. The method for preparing nitrate ester as claimed in claim 1 , wherein the flow rate for transferring the first ...

Method and Device for Removing Contaminants Arising During the Production of Aliphatic Nitrate Esters

The invention relates to a method and to a device for removing contaminants arising during the production of aliphatic or alicyclic nitric acid esters, in particular for removing contaminants from nitrated crude nitric acid esters, which nitrated crude nitric acid esters arise during the nitration of monovalent or multivalent aliphatic or alicyclic alcohols capable of nitration, after the separation of the final nitrating acid, and to a production system for nitrating monovalent or multivalent aliphatic alcohols capable of nitration with subsequent purification of the nitrated nitric acid esters. 115-. (canceled)16. A process for removing impurities obtained in the preparation of aliphatic or cycloaliphatic nitric esters ,wherein the process comprises removing impurities from crude nitric esters obtained in the nitration of nitratable monohydric or polyhydric aliphatic or cycloaliphatic alcohols, after removal of the residual nitrating acid, by treatment with at least one washing medium,wherein the process comprises the following process steps:(a) the crude nitric esters are firstly brought into contact with a washing medium, wherein the crude nitric esters and the washing medium are dispersed in one another in such a way that an emulsion results; and then(b) the resulting emulsion is subsequently fed into a tube reactor, which is equipped with mixing elements for introducing additional mixing energy, so that the impurities initially present in the crude nitric esters are at least partly removed during passage of the emulsion through the tube reactor, wherein the impurities initially present in the crude nitric esters are at least partly transferred into the washing medium and are neutralized thereby during passage of the emulsion through the tube reactor.17. The process as claimed in claim 16 ,wherein the nitric esters to be purified are selected from the group consisting of:(i) nitric esters of aliphatic or cycloaliphatic monoalcohols;(ii) nitric esters of ...

Production of fatty olefin derivatives via olefin metathesis

In one aspect, the invention provides a method for synthesizing a fatty olefin derivative. The method includes: a) contacting an olefin according to Formula I with a metathesis reaction partner according to Formula IIb in the presence of a metathesis catalyst under conditions sufficient to form a metathesis product according to Formula IIIb: and b) converting the metathesis product to the fatty olefin derivative. Each R 1 is independently selected from H, C 1-18 alkyl, and C 2-18 alkenyl; R 2b is C 1-8 alkyl; subscript y is an integer ranging from 0 to 17; and subscript z is an integer ranging from 0 to 17. In certain embodiments, the metathesis catalyst is a tungsten catalyst or a molybdenum catalyst. In various embodiments, the fatty olefin derivative is a pheromone. Pheromone compositions and methods of using them are also described.

Method and device for removing contaminants arising during the production of aliphatic nitrate esters

The invention relates to a method and to a device for removing contaminants arising during the production of aliphatic or alicyclic nitric acid esters, in particular for removing contaminants from nitrated crude nitric acid esters, which nitrated crude nitric acid esters arise during the nitration of monovalent or multivalent aliphatic or alicyclic alcohols capable of nitration, after the separation of the final nitrating acid, and to a production system for nitrating monovalent or multivalent aliphatic alcohols capable of nitration with subsequent purification of the nitrated nitric acid esters.

Method and device for removing contaminants arising during the production of aliphatic nitrate esters

The invention relates to a method and to a device for removing contaminants arising during the production of aliphatic or alicyclic nitric acid esters, in particular for removing contaminants from nitrated crude nitric acid esters, which nitrated crude nitric acid esters arise during the nitration of monovalent or multivalent aliphatic or alicyclic alcohols capable of nitration, after the separation of the final nitrating acid, and to a production system for nitrating monovalent or multivalent aliphatic alcohols capable of nitration with subsequent purification of the nitrated nitric acid esters.

一种废酸的处理方法

本发明涉及炼油助剂技术领域，尤其涉及一种废酸的处理方法。所述处理方法包括以下步骤：A)将生产硝酸异辛酯产生的废酸与三氧化硫在10～50℃下混合，混合后的废酸中，硫酸的质量浓度为90～97wt％；B)将所述混合后的废酸与硝酸按照质量比为2.7～6.0：1混合，得到混合酸；C)将所述混合酸与异辛醇按照质量比为1.2～2.7：1混合，反应后，得到的产物中的有机相经中和，得到硝酸异辛酯。本发明将生产硝酸异辛酯产生的废酸经上述处理，废酸得到了有效利用，无二次污染，成本较低，同时，可以制得产品硝酸异辛酯，无其他杂质带入，产品的质量较优。

Method of producing nano-capsules of ethyl nitrate

FIELD: nanotechnologies. SUBSTANCE: invention relates to nanotechnology, specifically to a method of producing nitric capsules of ethylnitrate. Method is characterized by that nanocapsules are represented by kappa-carrageenan and ethylnitrate as nucleus, wherein ethyl nitrate is slowly added to kappa-carrageenan suspension in toluene in presence of 0.01 g of E472c preparation as surfactant while stirring 800 rpm. Weight ratio of core:shell in terms of dry substance is 1:3, or 1:5, or 1:2. Then chloroform is added, obtained suspension is filtered and dried at room temperature. EFFECT: disclosed method enables to obtain nanitcapsules of ethylnitrate in a kappa-carrageenan shell. 1 cl, 3 ex РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2 697 252 C1 (51) МПК B82B 1/00 (2006.01) B82B 3/00 (2006.01) C07C 203/04 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ На основании пункта 1 статьи 1366 части четвертой Гражданского кодекса Российской Федерации патентообладатель обязуется заключить договор об отчуждении патента на условиях, соответствующих установившейся практике, с любым гражданином Российской Федерации или российским юридическим лицом, кто первым изъявил такое желание и уведомил об этом патентообладателя и федеральный орган исполнительной власти по интеллектуальной собственности. (52) СПК (21)(22) Заявка: 2018132092, 06.09.2018 (24) Дата начала отсчета срока действия патента: (73) Патентообладатель(и): Кролевец Александр Александрович (RU) Дата регистрации: 13.08.2019 (56) Список документов, цитированных в отчете о поиске: RU 2646482 C2, 05.03.2018. RU 2644725 C2, 13.02.2018. B.V.N. NAGAVARMA ET AL., Different techniques for preparation of polymeric nanoparticles, ASIAN J. PHARM. CLIN. RES., 2012, Vol. 5, Suppl. 3, 16-23. Приоритет(ы): (22) Дата подачи заявки: 06.09.2018 (54) Способ получения нанокапсул этилнитрата (57) Реферат: Изобретение относится к области нанотехнологии, конкретно к способу получения нанокапсул ...

Highly z-selective and enantioselective ring opening/cross metathesis

This invention relates generally to enantiomerically enriched C-H activated ruthenium olefin metathesis catalyst compounds which are stereogenic at ruthenium, to the preparation of such compounds, and the use of such catalysts in the metathesis of olefins and olefin compounds, more particularly, in the use of such catalysts in enantio- and Z-selective olefin metathesis reactions. The invention has utility in the fields of catalysis, organic synthesis, polymer chemistry, and industrial and fine chemicals chemistry.

一种废酸回用制备硝酸异辛酯的方法

本发明提供一种废酸回用制备硝酸异辛酯的方法，包括以下步骤：A)在废酸中加入98％的硫酸，得到硫酸浓度为90～95％的废酸；所述废酸中硫酸的质量浓度为80～85％，硝酸的质量浓度为2～6％；B)在所述硫酸浓度为90～95％的废酸中加入硝酸，得到混酸原料；所述混酸原料中，所述硝酸与所述步骤A)得到的硫酸浓度90～95％的废酸的质量比为1：(1.5～4)；C)将混酸原料和异辛醇打入微通道反应器内，进行反应，得到硝酸异辛酯。本发明中的废酸可以制得产品硝酸异辛酯，无其他杂质带入，产品的质量较优；且解决了含硝废酸后处理产生氮氧化物排放污染；废酸中的硝酸可再次使用，降低硝酸单耗。

制备单羟基醇的硝酸酯的方法

本发明涉及一种制备单羟基醇的硝酸酯的方法，其中在绝热反应条件下在硫酸存在下将单羟基醇或单羟基醇的混合物用硝酸转化成相应的硝基酯。

Способ получения нитратов одноатомных спиртов

ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß (19) RU (11) 2006 140 866 (13) A (51) ÌÏÊ C07C 201/00 (2006.01) ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÇÀßÂÊÀ ÍÀ ÈÇÎÁÐÅÒÅÍÈÅ (21), (22) Çà âêà: 2006140866/04, 20.11.2006 (30) Êîíâåíöèîííûé 21.11.2005 DE 30.11.2005 DE 30.11.2005 DE (71) Çà âèòåëü(è): ÉÎÇÅÔ ÌÀÉÑÑÍÅÐ ÃÌÁÕ ÝÍÄ ÊÎ. Êà (DE) ïðèîðèòåò: 102005055794.5 102005056974.9 102005057555.2 R U (57) Ôîðìóëà èçîáðåòåíè 1. Ñïîñîá ïîëó÷åíè íèòðàòîâ îäíîàòîìíûõ ñïèðòîâ, îòëè÷àþùèéñ òåì, ÷òî îäíîàòîìíûé ñïèðò èëè ñìåñü îäíîàòîìíûõ ñïèðòîâ ïîäâåðãàþò â àäèàáàòè÷åñêèõ óñëîâè õ â ïðèñóòñòâèè ñåðíîé êèñëîòû âçàèìîäåéñòâèþ ñ àçîòíîé êèñëîòîé. 2. Ñïîñîá ïî ï.1, îòëè÷àþùèéñ òåì, ÷òî â êà÷åñòâå îäíîàòîìíûõ ñïèðòîâ èñïîëüçóþò ïðåæäå âñåãî ïåðâè÷íûå îäíîàòîìíûå ñïèðòû, ïðåäïî÷òèòåëüíî Ñ4-Ñ12ñïèðòû, áîëåå ïðåäïî÷òèòåëüíî Ñ5-Ñ8ñïèðòû, ïðåæäå âñåãî èç ãðóïïû, âêëþ÷àþùåé àìèëîâûå ñïèðòû, ãåêñàíîë, ãåïòàíîë è îêòàíîë, à òàêæå èõ èçîìåðû è ñìåñè. 3. Ñïîñîá ïî ï.1 èëè 2, îòëè÷àþùèéñ òåì, ÷òî âçàèìîäåéñòâèå ïðîâîä ò â èíòåðâàëå òåìïåðàòóð îò 10 äî 80°Ñ, ïðåäïî÷òèòåëüíî îò 10 äî 70°Ñ, îñîáåííî ïðåäïî÷òèòåëüíî îò 20 äî 60°Ñ, ïðåäïî÷òèòåëüíî â íåïðåðûâíîì ðåæèìå. 4. Ñïîñîá ïî ï.1, îòëè÷àþùèéñ òåì, ÷òî âçàèìîäåéñòâèå ïðîâîä ò â ðåàêòîðå ïðè ïðîäîëæèòåëüíîñòè âçàèìîäåéñòâè (ðåàêöèè) îò 0,01 äî 30 ñ, ïðåäïî÷òèòåëüíî îò 0,1 äî 20 ñ, îñîáåííî ïðåäïî÷òèòåëüíî îò 0,1 äî 10 ñ. 5. Ñïîñîá ïî ï.1, îòëè÷àþùèéñ òåì, ÷òî ê ðåàêöèîííîé ñìåñè ïîäâîä ò ýíåðãèþ äë åå ïåðåìåøèâàíè èç ðàñ÷åòà 10-1000 Äæ/ë, ïðåäïî÷òèòåëüíî 10-300 Äæ/ë, îñîáåííî ïðåäïî÷òèòåëüíî 10-100 Äæ/ë. 6. Ñïîñîá ïî ï.1, îòëè÷àþùèéñ òåì, ÷òî ðàçäåë þò ôàçû îáðàçîâàâøåéñ â ðåçóëüòàòå âçàèìîäåéñòâè ñìåñè, êîòîðà ñîñòîèò èç îòðàáîòàííîé íèòðóþùåé êèñëîòû è ïðîäóêòà è êîòîðóþ ïîñëå âûõîäà èç ðåàêòîðà è ïåðåä ðàçäåëåíèåì ôàç ñíà÷àëà îõëàæäàþò äî òåìïåðàòóðû â èíòåðâàëå îò 10 äî 30°Ñ, ïðåäïî÷òèòåëüíî â èíòåðâàëå îò 15 äî 20°Ñ. 7. Ñïîñîá ïî ï.1, îòëè÷àþùèéñ òåì, ÷òî ñîîòíîøåíèå â èñõîäíîé ñìåñè ìåæäó àçîòíîé êèñëîòîé è ñåðíîé ...

Method for preparing nitrooxy-derivatives of naproxen

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to a method for synthesis of nitrooxy-derivatives of naproxen. Invention describes a method for synthesis of compound of the general formula (A) wherein R means compound of the formula: wherein R' means hydrogen atom or bromine (Br) atom; R 1 -R 12 are similar or different and mean independently hydrogen atom, linear or branched (C 1 -C 6 )-alkyl optionally substituted with aryl; each among m, n, o, p, q, r and s means independently a whole number from 0 to 6; p = 0 or 1; X means oxygen atom (O), sulfur (S) atom, -SO , -SO 2 , -NR 13 or -PR 13 wherein R 13 means hydrogen atom, (C 1 -C 6 )-alkyl; or X is chosen from group including: -cycloalkylene with 5-7 carbon atoms in cycloalkylene ring wherein ring is optionally substituted with side chains T wherein T means linear or branched alkyl with 1-10 carbon atoms; -arylene optionally substituted with one or more halogen atoms, linear or branched alkyl groups comprising from 1 to 4 carbon atoms, or linear or branched (C 1 -C 3 )-perfluoroalkyl; -5 or 6-membered saturated, unsaturated or aromatic heterocyclic ring chosen from formula X1-X13: . Indicated method involves: (i) adding reaction of compound of the formula (B): R-COOZ wherein R is given above; Z means hydrogen atom or cation chosen from Li + , Na + , Ca ++ , Mg ++ , tetraalkyl ammonium, tetraalkyl phosphonium with compound of the following formula (C): wherein R 1 -R 2 and m, n, o, p, q, r and s are given above; Y is chosen from halogen atom, -BF 4 , -SbF 6 , FSO 3- , R A SO 3- wherein R A means linear or branched (C 1 -C 6 )-alkyl optionally substituted with one or more halogen atoms, or (C 1 -C 6 )-alkylaryl; -R B COO - wherein R B means linear or branched (C 1 -C 6 )-alkyl, aryl optionally substituted with one or more halogen atoms or NO 2 -groups, (C 4 -C 10 )-heteroaryl and comprising one or more heteroatoms that are similar or different and chosen from nitrogen, oxygen, sulfur ...

Novel efficient cetane number improver and preparation method thereof

本发明公开一种新型高效柴油十六烷值改进剂的制备方法，属于炼油助剂技术领域。它是由硝酸和异辛醇在催化剂浓硫酸的作用下，在管式反应器中经混合段，反应段酯化而成。与传统十六烷值改进剂的制备工艺相比，本发明以硝酸、硫酸和异辛醇为起始原料，运用管式反应器进行管式反应，得到的产物采取加入片碱进行中和干燥过滤得到纯度较高的产品，成功解决了传统釜式硝化反应存在的安全隐患和生产效率低的问题，提高了产品纯度和收率，简化了产品的后处理。添加柴油中，可有效提高柴油的十六烷值性能。

Fuel composition for diesel engines

1. Топливная композиция для дизельных двигателей, отличающаяся тем, что в качестве присадки к дизельному топливу используется 10-25% мас. смеси алкилнитратов спиртов С-С, 10-25% мас. смеси простых диалкиловых эфиров изостроения на основе спиртов С-Си до 100% мас. дизельного топлива или любого углеводородного растворителя, причем в качестве исходных спиртов С-Сдля получениясмеси алкилнитратов и смеси простых диалкиловых эфировиспользуют фракцию спиртов C-C, полученных методом жидкофазного окисления фракции н-алканов C-Cводным раствором пероксида водорода в среде метанола на гетерогенном катализаторе ДП-2 и последующего гидрирования реакционной массы на жестком ячеистом катализаторе Pd/AlO.2. Дизельное топливо на основе базового топлива, содержащее присадку, отличающуюся тем, что оно содержит присадку по п. 1 в количестве 0,01-0,5% мас. РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2015 105 431 A (51) МПК C10L 10/00 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ЗАЯВКА НА ИЗОБРЕТЕНИЕ (21)(22) Заявка: 2015105431, 18.02.2015 Приоритет(ы): (22) Дата подачи заявки: 18.02.2015 (43) Дата публикации заявки: 10.09.2016 Бюл. № 25 A R U (57) Формула изобретения 1. Топливная композиция для дизельных двигателей, отличающаяся тем, что в качестве присадки к дизельному топливу используется 10-25% мас. смеси алкилнитратов спиртов С6-С9, 10-25% мас. смеси простых диалкиловых эфиров изостроения на основе спиртов С6-С9 и до 100% мас. дизельного топлива или любого углеводородного растворителя, причем в качестве исходных спиртов С6-С9 для получения смеси алкилнитратов и смеси простых диалкиловых эфиров используют фракцию спиртов C6-C9, полученных методом жидкофазного окисления фракции н-алканов C6-C9 водным раствором пероксида водорода в среде метанола на гетерогенном катализаторе ДП-2 и последующего гидрирования реакционной массы на жестком ячеистом катализаторе Pd/Al2O3. 2. Дизельное топливо на основе базового топлива, содержащее присадку, отличающуюся тем, что оно ...

Method of producing monohydric alcohol nitrates

FIELD: chemistry. SUBSTANCE: present invention refers to method of producing monohydric alcohol nitric acid esters. According to the method monohydric alcohol or mixed monohydric alcohols reacts with nitric acid in adiabatic conditions with sulphuric acid added. EFFECT: there is developed new method of producing the specified esters. 2 ex, 10 cl РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) 2 351 583 (13) C2 (51) МПК C07C 201/02 C07C 203/04 (2006.01) (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ, ПАТЕНТАМ И ТОВАРНЫМ ЗНАКАМ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ (21), (22) Заявка: 2006140866/04, 20.11.2006 (24) Дата начала отсчета срока действия патента: 20.11.2006 (43) Дата публикации заявки: 10.06.2008 (45) Опубликовано: 10.04.2009 Бюл. № 10 (54) СПОСОБ ПОЛУЧЕНИЯ СЛОЖНЫХ ЭФИРОВ АЗОТНОЙ КИСЛОТЫ ОДНОАТОМНЫХ СПИРТОВ (57) Реферат: Настоящее изобретение относится к способу получения сложных эфиров азотной кислоты одноатомных спиртов, согласно которому одноатомный спирт или смесь одноатомных спиртов подвергают в адиабатических условиях в присутствии серной кислоты взаимодействию с азотной кислотой. Технический результат: разработан новый способ получения указанных сложных эфиров. 9 з.п. ф-лы. R U 2 3 5 1 5 8 3 Адрес для переписки: 101000, Москва, М.Златоустинский пер., 10, кв.15, "ЕВРОМАРКПАТ", пат.пов. И.А.Веселицкой, рег. № 11 C 2 C 2 (56) Список документов, цитированных в отчете о поиске: RU 2235118 С1, 27.08.2004. RU 2259348 С1, 27.08.2005. US 5162568 А, 10.11.1992. DE 2039609 А1, 17.02.1972. Ñòðàíèöà: 1 ru 2 3 5 1 5 8 3 (73) Патентообладатель(и): ЙОЗЕФ МАЙССНЕР ГМБХ ЭНД КО. КГ (DE) R U (30) Конвенционный приоритет: 21.11.2005 DE 102005055794.5 30.11.2005 DE 102005056974.9 30.11.2005 DE 102005057555.2 (72) Автор(ы): ПЁЛЬМАНН Юрген (DE), ПОТТХАРСТ Франк (DE), ГЕРМАНН Генрих (DE), КОНЕЧНЫ Петер (DE), ХЭНДЕЛЬ Мирко (DE), ГЕБАУЕР Юрген (DE) RUSSIAN FEDERATION (19) RU (11) 2 351 583 (13) C2 (51) Int. Cl. C07C 201/02 C07C 203/04 (2006.01) (2006.01) FEDERAL SERVICE FOR ...

Preparation process of amantadine nitrate derivative

本发明公开了一种金刚烷胺类硝酸酯衍生物的制备工艺，其包括以取代或者未取代的金刚烷为原料，通过以下几步反应制备金刚烷胺类硝酸酯衍生物：(1)金刚烷醇的合成；(2)金刚烷醇的羧化；(3)金刚烷酸的酰胺化；(4)还原；(5)酰胺基金刚烷醇的水解与氨基的Boc保护；(6)Boc保护金刚烷胺醇的析晶；(7)Boc保护金刚烷胺醇的硝酸酯化；(8)硝酸酯化产物的精制；(9)氨基去保护与成盐；(10)金刚烷胺硝酸酯的精制。所述金刚烷胺类硝酸酯衍生物为： 其中，R 1 ，R 2 相同或不相同，分别为氢，直链或支链烷基，取代或未取代的芳基，芳杂基。本发明提供了一种高效、经济、绿色、安全、可靠并且适于工业化生产的金刚烷胺硝酸酯衍生物的制备工艺。

Recovery of nitrated compounds using solvent extraction and distillation

A method for separating an aqueous solution which contains minor amounts of nitrated esters which are only slightly soluble in water is provided. Separation of the nitrated esters, which include ethylene glycol dinitrate and nitroglycerin, is effected by contacting the aqueous solution with an organic phase of ethylene glycol dinitrate for a period of time sufficient to allow extraction of the nitroglycerin in solution into the ethylene glycol dinitrate phase. The organic ethylene glycol dinitrate phase is then separated from the aqueous solution, and the latter is distilled at a temperature of from about 50 degrees F. to about 200 degrees F. at a lower than atmospheric pressure. Upon completion of the separation process water, which is substantially free of nitrated esters, is suitable for discharge and return to a natural environment.

Process for preparing nitrooxyderivatives of naproxen

본 발명은 화학식 (B)의 화합물을 화학식 (C)의 화합물과 반응시키는 것을 포함하여, 화학식 (A)의 화합물을 제조하는 방법에 관한 것이다: R-COOZ (B) 상기 식에서, R은 나프록센 또는 브로모나프록센의 기이며, R 1 -R 12 는 수소, 또는 알킬 그룹이고, m, n, o, q, r 및 s는 각각 독립적으로 0 내지 6의 정수이고, p는 0 또는 1이고, X는 O, S, SO, SO 2 , NR 13 또는 PR 13 , 또는 아릴, 헤테로아릴 그룹이고, Z는 수소, 또는 Li+, Na+, K+, Ca++, Mg++, 테트라알킬암모늄 및 테트라알킬포스포늄으로부터 선택된 양이온이고; Y는 적합한 이탈기이다. 2-(S)-(5-브로모-6-메톡시-2-나프틸)-프로파노산, 4-(니트로옥시)부틸 에스테르, 나프록센, 브로모나프록센

Method for preparing isooctyl nitrate in micro-channel reactor

本发明公开了一种在微通道反应器中制备硝酸异辛酯的方法，以异辛醇、硝硫混酸为原料，不使用任何惰性溶剂及添加剂，将反应原料在微通道反应器中进行反应。本发明利用微反应器超强的换热能力，解决了局部反应过热的问题，避免了使用大规模的冷却系统，降低了能耗；反应后的硝硫混酸经过简单的处理即可重复使用；同时避免了反应中惰性溶剂或者稳定剂等的加入和反应后的分离问题，简化了生产工艺的同时，节约了物料，又进一步降低了分离所带来的能耗问题，制得的硝酸异辛酯产品不需要任何蒸馏等提纯手段处理纯度可达99.0％以上。

Method for continuously synthesizing isooctyl nitrate and extracting residual acid in isooctyl nitrate in microreactor

一种在微反应器中连续合成硝酸异辛酯并萃取其中残余酸的方法，以异辛醇和硫/硝摩尔比为1.5～2.5的混酸为原料在第一微反应器通过硝化反应，生成硝酸异辛酯和废酸，经液‑液自动分离器分离出含酸的硝酸异辛酯粗品；该粗品与NaOH水溶液在第二微反应器内混合，进而反应萃取其中的残余酸，水油分离后得到酸含量极低的硝酸异辛酯。萃取效率高于96％。本发明实现了硝酸异辛酯合成与除酸的连续化操作，降低了危险等级且减少了除酸耗时、提高了生产效率。

Process for the removal of impurities resulting from the production of aliphatic nitrate esters

Verfahren zur Entfernung von bei der Herstellung von aliphatischen oder cycloaliphatischen Salpetersäureestern (Nitratestern) anfallenden Verunreinigungen, insbesondere zur Entfernung von Verunreinigungen aus bei der Nitrierung von nitrierbaren ein- oder mehrwertigen aliphatischen oder cycloaliphatischen Alkoholen nach Abtrennung der Nitrierendsäure anfallenden Rohsalpetersäureestern, durch Behandlung mit mindestens einem Waschmedium, wobei das Verfahren die folgenden Verfahrensschritte umfasst: (a) zunächst werden die Rohsalpetersäureester mit einem Waschmedium in Kontakt gebracht, wobei die Rohsalpetersäureester und das Waschmedium derart ineinander verteilt werden, dass eine Emulsion resultiert; und (b) nachfolgend wird die resultierende Emulsion in einen Rohrreaktor einspeist, wobei der Rohrreaktor mit Mischelementen, insbesondere zum Eintrag von zusätzlicher Mischenergie, ausgestattet ist, so dass während des Durchtritts der Emulsion durch den Rohrreaktor die in den Rohsalpetersäureestern anfänglich vorhandenen Verunreinigungen zumindest teilweise entfernt werden und/oder so dass während des Durchtritts der Emulsion durch den Rohrreaktor die in den Rohsalpetersäureestern anfänglich vorhandenen Verunreinigungen zumindest teilweise in das Waschmedium überführt und/oder hierdurch neutralisiert werden. Process for removing impurities resulting from the production of aliphatic or cycloaliphatic nitric acid esters (nitrate esters), in particular for removing impurities from crude nitric esters resulting from the nitration of nitratable monohydric or polyhydric aliphatic or cycloaliphatic alcohols after removal of the nitrating acid by treatment with at least one washing medium wherein the method comprises the following steps: (a) first the crude nitric acid esters are contacted with a washing medium, wherein the crude nitric acid esters and the washing medium are distributed into each other such that an emulsion results; and (b) subsequently, the resulting emulsion ...

Nitrate ester of ether of glycerol and ethanol as a cetane improver for diesel and its preparation

本発明は、ディーゼル用セタン価向上剤としてのグリセロール及びエタノールのエーテルの硝酸エステルの使用及びその製造プロセスに関するものであり、バイオディーゼル製造から得られるグリセロールから添加剤を製造すること、及びディーゼルの点火を促進しディーゼル燃料のセタン価を向上させるためのより経済的かつ効率的な選択肢を添加剤市場にもたらすことを目的とする。【選択図】図１

Process for producing latanoprosten-bunod and its intermediates, and compositions containing them

METHOD FOR CLEANING 4- (NITROXY) BUTYL (2S) -2- (6-METHOXY-2-NAPTIL) PROPANOATE

1. Способ очистки напроксинода, включающий следующие стадии: ! a) растворение или диспергирование смеси, содержащей напроксинод, в растворителе; ! b) охлаждение раствора или двухфазной дисперсии при перемешивании до температуры от -20°С до 10°С; ! c) необязательная затравка раствора кристаллами напроксинода; ! d) перемешивание при температуре в диапазоне от -40°С до 10°С; ! e) сбор образовавшегося твердого вещества при температуре ниже 15°С; ! 2. Способ по п.1, где смесь содержит напроксинод в количестве выше 90 вес.%. ! 3. Способ по п.1, где растворитель на стадии а) представляет собой полярный протонный растворитель, или апротонный растворитель, или их смесь. ! 4. Способ по п.3, где полярный протонный растворитель выбирают из спиртов, диолов, амидов, или их смесей. ! 5. Способ по п.4, где полярным протонным растворителем является метанол, этанол, изопропанол или 1-бутанол, диэтиленгликоль или формамид, или их смесь. ! 6. Способ по п.5, где температура на стадии b) находится в диапазоне от -15°С до 5°С. ! 7. Способ по п.6, где температура на стадии d) находится предпочтительно в диапазоне от -15°С до 5°С. ! 8. Способ по п.7, где температура на стадии е) составляет ниже 10°С. ! 9. Способ по п.2, где растворитель на стадии а) представляет собой полярный протонный растворитель, или апротонный растворитель, или их смесь. ! 10. Способ по п.9, где полярный протонный растворитель выбирают из спиртов, диолов, амидов, или их смесей. ! 11. Способ по п.10, где полярным протонным растворителем является метанол, этанол, изопропанол или 1-бутанол, диэтиленгликоль или формадид, или их смеси. ! 12. Способ по п.11, где температура на стадии в) находится в диапазоне от -15°С до 5°С. ! 13. Спосо� РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) 2010 120 745 (13) A (51) МПК C07C 203/04 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ЗАЯВКА НА ИЗОБРЕТЕНИЕ (71) Заявитель(и): НИКОКС С.А. (FR) (21)(22) Заявка: 2010120745/04, 18.06.2009 Приоритет(ы): (30) Конвенционный приоритет: 20. ...

Halogen alkyl nitrate synthesis method

FIELD: chemistry. ^ SUBSTANCE: described is a stable non-explosive composition which contains a) a compound of formula (I): Br-(CH2)4-ONO2 and b) CH2Cl2 as a solvent. The formula (I) compound is present in concentration not greater than 20 wt %. Described is a method of preparing the said composition, involving slow addition of a compound of formula (II): Br-(CH2)4-OH (II), to a nitrating agent selected from a group consisting of concentrated nitric acid/concentrated sulphuric acid with molar ratio 1:1 (sulphonitrating mixture), and to CH2Cl2. ^ EFFECT: design of an efficient halogen alkyl nitrate synthesis method. ^ 3 cl, 1 tbl, 5 ex РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) 2 388 746 (13) C2 (51) МПК C07C 201/08 C07C 205/08 (2006.01) (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ, ПАТЕНТАМ И ТОВАРНЫМ ЗНАКАМ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ (21), (22) Заявка: 2007118914/04, 09.11.2005 (24) Дата начала отсчета срока действия патента: 09.11.2005 (72) Автор(ы): РИВОЛТА Романо (IT), ФИНЛАНДЕР Петер (DK) (43) Дата публикации заявки: 27.12.2008 2 3 8 8 7 4 6 (45) Опубликовано: 10.05.2010 Бюл. № 13 (56) Список документов, цитированных в отчете о поиске: J. MED. CHEM., vol.36, 1993, 815-819. Журнал органической химии, т.4, №11, 1968, 1893-1899. CHEM. PHARM. BULL., vol.41, № 6, 1993, 1049-1054. 2 3 8 8 7 4 6 R U (86) Заявка PCT: EP 2005/055865 (09.11.2005) C 2 C 2 (85) Дата перевода заявки PCT на национальную фазу: 25.06.2007 (87) Публикация PCT: WO 2006/056535 (01.06.2006) Адрес для переписки: 121087, Москва, а/я 33, пат.пов. В.В.Курышеву, рег.№ 0006 (54) СПОСОБ ПОЛУЧЕНИЯ ГАЛОГЕНАЛКИЛНИТРАТОВ добавление соединения формулы (II): Br-(СН2)4ОН (II), к нитрующему агенту, выбранному из группы, состоящей из концентрированной азотной кислоты/концентрированной серной кислоты с молярным соотношением 1:1 (сульфонитрующая смесь), и к CH2Cl2 . 2 н. и 1 з.п. ф-лы, 1 табл. (57) Реферат: Описана стабильная композиция, не являющаяся взрывоопасной, содержащая а) соединения ...

Method for producing organic nitro compounds

FIELD: chemistry. SUBSTANCE: invention relates to the organic nitro compound chemistry and specifically to a process for producing nitro compounds of the general formula of RNO 2 , where R=n-C 4 H 9 O-; O 2 NO(CH 2 ) 2 O-; O 2 NO(CH 2 ) 2 O(CH 2 ) 2 O-; O 2 NOCH 2 CH(ONO 2 )CH 2 O-; (O 2 NOCH 2 ) 3 CCH 2 O-; where m=1, 2; where n=2, 3; , which can find application in producing high-energy products, medicines, dyes, polymers, etc. The method consists in the fact that the corresponding alcohols or amines derivatives are subject to nitration with nitric oxide (V) or its mixture with 100% nitric acid in a medium of lower hydrofluorocarbons, the process is carried out at a pressure of 3-60 bar and a temperature of 5-40°C at a molar ratio of the corresponding starter compound and nitrating agent 1:(1.1-4.4). EFFECT: method allows to reduce fire and explosion hazard of the process, improve its environmental performance and obtain the desired compounds with high output. 2 cl, 20 ex РОССИЙСКАЯ ФЕДЕРАЦИЯ ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ФОРМУЛА (21)(22) Заявка: (19) RU (51) МПК C07C 201/02 C07C 203/04 C07C 241/00 C07C 243/02 C07D 233/02 C07D 239/04 C07D 493/04 2016112861, 05.04.2016 05.04.2016 Дата регистрации: C1 (2006.01) (2006.01) (2006.01) (2006.01) (2006.01) (2006.01) (2006.01) (72) Автор(ы): Жарков Михаил Николаевич (RU), Кучуров Илья Григорьевич (RU), Фоменков Игорь Владимирович (RU), Злотин Сергей Григорьевич (RU) (73) Патентообладатель(и): Федеральное государственное бюджетное учреждение науки Институт органической химии им. Н.Д. Зелинского Российской академии наук (ИОХ РАН) (RU) Приоритет(ы): (22) Дата подачи заявки: 05.04.2016 (45) Опубликовано: 17.02.2017 Бюл. № 5 (56) Список документов, цитированных в отчете о поиске: I.V. KUCHUROV ET AL., Synthesis of nitric acid esters from alcohols in a dinitrogen pentoxide/carbon dioxide liquid system, MENDELEEV COMMUN., 2012, 22, pp.67-69. I.V. KUCHUROV ET AL., Nitration of carbonic, sulfuric and ...

Safe method for obtaining dinitrate of vicinal glycols

FIELD: chemistry. SUBSTANCE: invention relates to chemical engineering and specifically to a method of producing dinitrates of vicinal 1,2-glycols which can be used as components of explosive compositions, solvents and medical preparations. Method consists in that initial 1,2-glycols at the first stage are sulphated with concentrated (95–97 wt. %) sulfuric acid with formation of corresponding acid sulphates with their further treatment at the second stage with sulfur-nitrogen nitrating mixture in presence of organochlorine solvents. EFFECT: disclosed method increases safety of the process of producing dinitrates of 1,2-glycols. 4 cl, 2 tbl РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2 688 690 C2 (51) МПК C07C 201/02 (2006.01) C07C 203/04 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ (52) СПК C07C 201/02 (2018.08) (21)(22) Заявка: 2017138019, 31.10.2017 (24) Дата начала отсчета срока действия патента: Дата регистрации: 22.05.2019 (43) Дата публикации заявки: 06.05.2019 Бюл. № 13 (45) Опубликовано: 22.05.2019 Бюл. № 15 0129995 A2, 02.01.1985. US 8658818 B2, 25.02.2014. (54) Безопасный способ получения динитратов вицинальных гликолей (57) Реферат: Изобретение относится к химической серной кислотой с образованием технологии, а именно к способу получения соответствующих кислых сульфатов с динитратов вицинальных 1,2-гликолей, которые последующей их обработкой на второй стадии могут найти применение в качестве компонентов серно-азотной нитрующей смесью в присутствии взрывчатых составов, растворителей и хлорорганических растворителей. Предлагаемый медицинских препаратов. Способ заключается в способ позволяет повысить безопасность том, что исходные 1,2-гликоли на первой стадии процесса получения динитратов 1,2-гликолей. 3 сульфатируют концентрированной (95-97 мас.%) з.п. ф-лы, 2 табл. R U 2 6 8 8 6 9 0 (56) Список документов, цитированных в отчете о поиске: RU 2567236 C1, 10.11.2015. EP Стр.: 1 C 2 C 2 Адрес для переписки: ...

Manufacturing process of amantadine-based nitrate derivatives

Nitration of organic compounds

ABSTRACT Nitration of organic compounds. Organic nitrogen compounds are formed in the vapour phase by organic radical formation by reaction of an organic compound, suitably an alkane, with hydroxyl radicals derived from the reaction between hydrogen peroxide and nitrogen dioxide and the nitration of the organic radicals, suitably with nitrogen dioxide. The process is conducted using a molecular oxygen additive which directs the reaction towards the formation of the nitrate corresponding to the organic compound which may predominate in the organic reaction products.

Production of fatty olefin derivatives via olefin metathesis

The invention provides a method for synthesizing a fatty olefin derivative. In some embodiments, the method includes: a) contacting an unsaturated olefin with an unsaturated fatty acid ester in the presence of a metathesis catalyst under conditions sufficient to form a metathesis product and b) converting the metathesis product to the fatty olefin derivative. In certain embodiments, the metathesis catalyst is a tungsten catalyst or a molybdenum catalyst. In various embodiments, the fatty olefin derivative is an insect pheromone. Pheromone compositions and methods of using them are also described.

Improvements in the preparation of propyl nitrate

Nitration of alkanols

A process for nitrating alkanols containing 5-13 carbon atoms is disclosed. The nitation takes place at 15°-45° C. using a mixed acid containing 20-30% nitric acid, 55-60% sulfuric acid and 15-20% water, and 2-5%, based on mixed acid, of a stabilizer selected from the class consisting of urea, sulfamic acid and hydrazine.

Process for the preparation of 1-oxo-2-nitratocycloalkanes

Crystallisation of pentacrythritol tetranit - rate

Pentaerythritol tetranitrate (PETN), is obtained as freely flowing crystals by stirring an aqs. acetone (pref.) solution of PETN containing 0.1-10% of a higher homologue. The latter may be dipentaerythritol hexanitrate, tripentaerythritol octonitrate and/or tetrapentaerythritol decanitrate. Soft crystals may be obtd. at 25-35 degrees C, hard, large crystals at 60-65 degrees C and small crystals from well-stirred solutions. Explosive properties e.g. detonation speed are better than for PETN previously produced.

METHOD FOR PRODUCING HALOGENALKylNITRATES

1. Раствор, содержащийа) соединение общей формулы (I):,где Х представляет собой атом галогена, выбранный из Cl, Br, I;n является целым числом от 3 до 6; иб) растворитель, выбранный из группы, состоящей из CHCl, CHCl, CCl, перфторгексана, перфторгептана;отличающийся тем, что соединение формулы (I) присутствует в концентрации не более 20 вес.%.2. Раствор по п.1, содержащий соединение формулы (I), где n обозначает 4.3. Раствор по п.1, содержащий соединение формулы (I), где Х представляет собой Br.4. Раствор по п.1, где растворитель представляет собой СНCl.5. Раствор по любому из пп.1-4, где соединение формулы (I) присутствует в концентрации от 10 до 20 вес.%.6. Способ получения соединения формулы (I) по п.1, который включает медленное добавление соединения формулы (II):где Х и n являются такими, как определено в п.1,к нитрующему агенту, выбранному из группы, состоящей из концентрированной азотной кислоты/концентрированной серной кислоты (сульфонитрующая смесь), азотной кислоты отдельно, NaNOв трифторуксусной кислоте, солей нитрония, таких как NOBF, и к органическому растворителю, выбранному из группы, состоящей из CHCl, CHCl, CCl, перфторгексана, перфторгептана.7. Способ по п.6 для получения соединения формулы (I), где Х представляет собой Br.8. Способ по п.6 или 7, где органический растворитель представляет собой CHCl. ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß (19) RU 2007 118 914 (11) (13) A (51) ÌÏÊ C07C 201/08 (2006.01) ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÇÀßÂÊÀ ÍÀ ÈÇÎÁÐÅÒÅÍÈÅ (21), (22) Çà âêà: 2007118914/04, 09.11.2005 (71) Çà âèòåëü(è): ÍÈÊÎÊÑ Ñ.À. (FR) (30) Êîíâåíöèîííûé ïðèîðèòåò: 25.11.2004 EP 04292785.5 (43) Äàòà ïóáëèêàöèè çà âêè: 27.12.2008 Áþë. ¹ 36 (72) Àâòîð(û): ÐÈÂÎËÒÀ Ðîìàíî (IT), ÔÈÍËÀÍÄÅÐ Ïåòåð (DK) (87) Ïóáëèêàöè PCT: WO 2006/056535 (01.06.2006) Àäðåñ äë ïåðåïèñêè: 121087, Ìîñêâà, à/ 33, ïàò.ïîâ. Â.Â.Êóðûøåâó, ðåã.¹ 0006 R U (57) Ôîðìóëà èçîáðåòåíè 1. Ðàñòâîð, ñîäåðæàùèé à) ñîåäèíåíèå îáùåé ôîðìóëû (I): , ãäå Õ ...

PROCESS FOR RECOVERING NITRAL DERIVATIVES OF VERSATILE ALCOHOLS, FROM EFFLUENTS FROM THE PRODUCTION OF EXPLOSIVES CONTAINING NITROGLYCERINE

Blasting oil contained in the effluent from the production of explosives containing nitroglycerine is recovered by extracting with nitroaromatics which make part of the final explosive, the resulting extract being used completely in the explosive production. Residues of nitroaromatics may be removed from the purified effluent by means of an extraction liquid being sparely water-soluble, such as toluene or xylene or a mixture thereof.

Organic nitrate bile acid inclusion compounds

Inclusion compounds of bile acids and organic nitrates selected from glyceryl trinitrate, penta-erythritol tetranitrate, mannitol hexanitrate, erythritol tetranitrate and isosorbide dinitrate. Complexes are readily absorbed from the gastro-intestinal tract. The organic nitrates above are mainly used in treatment of angina pectoris. Solution of bile acid and organic nitrate in inert solvent which dissolves both. Product crystallises. Preferred molar ratio of nitrate:bile acid is 1:2. Desoxycholic acid (2.35 g.) and PETN (316 mg) were dissolved in 20 ml. of a 1:1 mixture of methanol and benzene with warming. The soln. was cooled to 0 deg.C and the crystals which separated were collected to give a PETN/desoxycholic acid complex with a ratio of 1:2. The mother liquors gave a mixture of inclusion compounds having a PETN/bile acid ratio of from 3:1 to 6:1.

Process for preparing nitrooxyderivatives of naproxen

本发明涉及制备通式(A)化合物的方法，其中R是萘普生或溴萘普生的基团，且R 1 －R 12 是氢或烷基，m、n、o、q、r和s分别独立地为0－6的整数，且p是0或1，且X是O、S、SO、SO 2 、NR 13 或PR 13 或芳基、杂芳基，所述方法包括将式(B)化合物：R－COOZ，其中R如上所定义，且Z是氢或选自下列的阳离子：Li+、Na+、K+、Ca++、Mg++、四烷基铵、四烷基鏻；与如说明书中所示的式(C)化合物反应，其中R 1 －R 12 和m、n、o、p、q、r、s如上所定义，且Y是合适的离去基团。

Process for preparing nitrooxyderivatives of naproxen

The present invention refers to a process for preparing a compound of general formula (A), wherein R is a radical of naproxen or bromonaproxen and R1-R12 are hydrogen or alkyl groups, m, n, o, q, r and s are each independently an integer from 0 to 6, and p is 0 or 1, and X is O, S, SO, SO2, NR13 or PR13or an aryl, heteroaryl group, said process comprising reacting a compound of formula (B) : R-COOZ wherein R is as defined above and Z is hydrogen or a cation selected from: Li+, Na+, K+, Ca++, Mg++, tetralkylammonium, tetralkylphosphonium, with a compound of formula (C), as reported in the description, wherein R1-R12 and m, n, o, p, q, r, s are as defined above and Y is a suitable leaving group.

Continuous manufacture of liquid and explosive nitric esters

PROCESS AND PLANT FOR DEGRADATION OF NITROGLYCERIN IN NITRATION RESIDUAL ACIDS

A continuous process for the degradation of nitroglycerine in the residual aclds from glycerol nitration comprises adding water or dilute sulphuric acid to the residual acids to improve the solubilisation of the nitroglycerine and then passing the residual acids to a plant comprising a circulating loop which comprises successively, in the direction of circulation of the acids, an inlet for the acids after addition of water or dilute sulphuric acid, an external microwave heating system for the acids, an outlet for the mixture thus treated, and an outlet for nitrous fumes. The invention also provides plant for carrying out this process.

Process for manufacturing nitroglycerin

Improvements in the manufacture of nitroglycerin

Patent FR2235110A1

A process for treating final acid obtained in forming a nitrate of a polyhydric alcohol, said final acid comprising a mixture of sulfuric acid, nitric acid, water and said nitrate, said process comprising mixing said final acid with an aromatic nitro compound, allowing said mixture to stratify whereby said nitrate is dissolved into said aromatic nitro compound as one layer and there is another substantially nitrate-free waste acid layer comprising sulfuric acid, nitric acid and water, and separating said layers. Preferably the nitrate is trinitroglycerine and the aromatic nitro compound is dinitrotoluene. The waste acid layer advantageously is partially used to form additional dinitrotoluene and is partially mixed with fresh final acid since its presence serves to stabilize such final acid by preventing any settling out of trinitroglycerine, presumably by the action of the small amount of dinitrotoluene which may be present in said waste acid.

Process for the production of cycloaliphatic nitrates

Manufacture of alkyl nitrates from alkylenes

Process for preparing monomitrochlorobenzene

ABSTRACT The invention is concerned with water dilutable binders for air drying coating compositions, the content of auxiliary organic solvent of which lies below 15 % of binder solids. One object of the invention is the use of such binders in the formulation of air drying paints which are useful for industrial applications for use by both professional and "do-it-yourself" painters. Another object is the formulation of force-drying coating composi-tions and, in conjunction with hardening components such as amine or phenolic resins, for stove paints. The binders consist of partial condensation products of:-(A) 30 - 70 % by weight of a film forming fatty acid modified alkyd resin intermediate with an acid value of be-tween 30 and 200 mg KOH/g, an intrinsic viscosity ?A of from 4.5 to 8 ml/g and an oil length of from 5 to 60 %, with (B) 70 - 30 % by weight of a film forming fatty acid modified alkyd resin intermediate with an acid valve of below 5 mg KOH/g, a hydroxyl value of from 50 to 300 mg KOH/g, an intrinsic viscosity ?B of from 8 to 12 ml/g and an oil length of from 5 to 60 %. the ratio between the intrisic viscosities lying between 1.4 to 2.7. Owing to the favourable gradient of the dilution curve, solutions are obtained which have a high solids content and are ready for application. PROCESS FOR PREPARING MONONITROCHLOROBENZENE ABSTRACT OF THE DISCLOSURE In a process for the preparation of mono-nitrochlorobenzene by nitration of chlorobenzene using a mixed acid of nitric acid and phosphoric acid, the nitration reaction is carried out by using a molar ratio of nitric acid to chlorobenzene of not more than equimol in the presence of a concentrated phosphoric acid as the phosphoric acid component at temperatures of 50°-120°C while maintaining the concentration of phosphoric acid to 72.4 weight % as P2O5 or more during the reaction.

Process for the preparation of latanoprostene bunod and intermediate thereof and compositions comprising the same

Processes for preparing latanoprostene bunod and an intermediate prepared from the process. Also latanoprostene bunod compositions having high-purity latanoprostene bunod.

Improvements in the manufacture of amyl nitrate

Continuous synthesis of isooctyl nitrate in a flow reactor

A process for synthesizing isooctyl nitrate in a continuous flow reactor comprises flowing a H2SO4-HNO3 mixture within a flow reactor, flowing isooctyl alcohol into said flow reactor so as to mix the isooctyl alcohol with the H2SO4-HNO3 mixture and produce a reaction mixture stream flowing in said reactor, maintaining the reaction mixture stream flowing in said flow reactor at a reaction temperature within in the range -10° to 35°C inclusive, and wherein the residence time of the reaction mixture stream in the flow reactor is greater than or equal to 5 seconds and less than or equal to 40 seconds, and wherein the H2SO4 of the H2SO4-HNO3 mixture is H2SO4 having a concentration of in the range of 85 to 95% inclusive, more desirably 88 to 92% inclusive, most desirably of 90%.

Process of producing the esters of nitric acid

Esters of nitric acid, for example, nitroglycerine and nitroglycol, are obtained by carrying out the esterification at low temperatures under reduced pressure, so that the water formed in the reaction evaporates.

And merritt t

Water removal in nitration of aromatic hydrocarbons

TITLE Water Removal in Nitration of Aromatic Hydrocarbons ABSTRACT OF THE DISCLOSURE The invention relates to a process for the preparation of nitrated aromatic compounds by the mixed acid process, in which water is removed from the re-action mass by passing an inert gas through it.

A process for obtaining (nitroxymethyl)phenyl esters of salicylic acid derivatives

A process for obtaining (nitroxymethyl)phenyl esters of salicylic acid derivatives of formula (I) wherein R1 is the OCOR3 group characterized in that it comprises the following steps: a) reaction of a halide of a salicylic acid derivative with hydroxybenzylalcohol in the presence of a base; b) nitration of the obtained product in anhydrous conditions by a mixture of nitric acid with a different inorganic acid, or an organic acid, or an anhydride of one or two organic acids; c) recovery of the final product.

Manufacture of nitric acid esters

540,050. Alkyl nitrates. STEVENS, A. H. (Sharples Solvents Corporation). March 29, 1940, No. 5722. Drawings to Specification. [Class 2 (iii)] Alkyl nitrates are produced by reacting in alcohol with nitric acid of 35-68 per cent. strength under a pressure of 20-650 mm., the nitrate being removed by azeotropicdistillation, water (or in the case of ethyl or methyl nitrate, the ester) being returned from the distillate or otherwise to the reaction vessel to prevent accumulation of ester or water. The invention is applicable to the esterification of dihydric alcohols. Urea is preferably added during the process, and the water to be returned may be added in the form of solvent or diluent of the nitric acid, urea or alcohol. Examples 1-11 describe the esterification of n-butyl, 2-chlorethyl, mixed amyl, secondary amyl, iso-amyl, n-amyl, n-hexyl, secondary hexyl, 2-ethoxyethyl, cyclohexyl, and octyl nitrates, using the reagents in the liquid phase. The alcohol may be supplied in the liquid or vapour phase. Another example describes the production of isopropyl nitrate, the alcohol being supplied in the form of vapour above the surface of the nitric acid. Specification 379,312 is referred to.

Process for the production of high energy material

ABSTRACT A process for the production of a high energy nitrate ester involves reacting, in an inert organic solvent, a heterocyclic compound, selected from oxiranes, oxetanes, N-substituted aziridines and N-substituted azetidines, with either N2O4 or N2O5, and when the compound is reacted with N2O4, oxidising the O- or N-nitrate sub-stituents or substituent in the product to O- or N-nitrate substituent or substituents. The remaining ring carbon atoms on the hetero-cyclic compound may be substituted or unsubstituted. Preferred substituent groups for the C and/or N ring atoms on the compound include alkyl, cyano alkyl, haloalkyl, nitroalkyl, and substituted aryl. Several novel nitrate esters are also provided, including nitrated derivatives of polybutadiene, in which between 1% and 25% of the carbon atoms in the polymer are substituted by vicinal nitrate ester (-ONO2) groups.

PROCESS AND PLANT FOR DEGRADATION OF NITROGLYCERIN IN NITRATION RESIDUAL ACIDS

L'invention se rapporte à un procédé et à une installation de dégradation de la nitroglycérine dans les acides résiduaires issus de la nitration de la glycérine. Le procédé selon l'invention consiste à traiter thermiquement ces acides résiduaires par micro-ondes et permet de récupérer séparément des acides concentrés. Le procédé consiste à ajouter de l'eau ou de l'acide sulfurique dilué dans les acides résiduaires pour améliorer la solubilité de la nitroglycérine et à faire circuler ces acides résiduaires dans une installation constituée par un circuit de circulation comprenant successivement dans le sens de circulation des acides, une entrée desdits acides après addition d'eau ou d'acide sulfurique dilué, un système de chauffage par micro-ondes des acides, une sortie du mélange ainsi traité, et une sortie des vapeurs nitreuses. The invention relates to a method and to an installation for degrading nitroglycerin in the residual acids resulting from the nitration of glycerin. The process according to the invention consists in thermally treating these residual acids by microwave and makes it possible to separately recover concentrated acids. The process consists in adding water or sulfuric acid diluted in the residual acids to improve the solubility of the nitroglycerin and in circulating these residual acids in an installation constituted by a circulation circuit comprising successively in the direction of circulation acids, an inlet of said acids after addition of water or dilute sulfuric acid, a microwave heating system for the acids, an outlet of the mixture thus treated, and an outlet of the nitrous vapors.

METHOD FOR PRODUCING ENERGY MATERIALS.

Patent FR2096179A5

1315053 Fluoroalcohols FARBWERKE HOECHST AG 9 June 1971 [10 June 1970] 19700/71 Heading C2E Compounds of formula R f CH 2 CH 2 OH, in which Rf is a C 4-16 -perfluoroalkyl group, are prepared by reaction of an iodide R f CH 2 CH 2 I with nitric acid to give a nitrate and subjecting this to catalytic hydrogenation. The compounds C 6 F 13 CH 2 CH 2 ONO 2 and C 6 F 13 CH 2 CH 2 ONO are prepared in comparative examples by reaction of the compound with nitric acid, or with sodium nitrite and sulphuric acid.

Patent SU367595A3

1315053 Fluoroalcohols FARBWERKE HOECHST AG 9 June 1971 [10 June 1970] 19700/71 Heading C2E Compounds of formula R f CH 2 CH 2 OH, in which Rf is a C 4-16 -perfluoroalkyl group, are prepared by reaction of an iodide R f CH 2 CH 2 I with nitric acid to give a nitrate and subjecting this to catalytic hydrogenation. The compounds C 6 F 13 CH 2 CH 2 ONO 2 and C 6 F 13 CH 2 CH 2 ONO are prepared in comparative examples by reaction of the compound with nitric acid, or with sodium nitrite and sulphuric acid.

Process for the preparation of naproxene-nitroxyalkyl ester, and such compound

4-nitroxybutyl ester of the 2-(S)-(6-methoxy-2-naphthyl)-propanoic acid having an enantiomeric excess of the (S) form higher than or equal to 97%.

Method for purifying 4-(nitrooxy)butyl(2s)-2-(6-methoxy-2-naphthyl)propanoate

The present invention relates to a method for purifying naproxcinod comprising the steps of : a) dissolving or dispersing a mixture containing naproxcinod in an amount higher than 90% by weight in a solvent; b) cooling the solution or two phases dispersion under stirring to a temperature ranging from -20°C to 10°C c) optionally seeding the solution with crystals of naproxcinod d) stirring, by maintaining the temperature in the range from - 40°C to 10°C e) collecting the formed solid by maintaining the temperature under 15°C A further object of the invention is a crystalline form of naproxcinod.

Process for the production of isopropyl nitrate

Process for producing energy-rich materials

L'invention concerne la fabrication de matériaux riches en énergie. Elle se rapporte à un procédé comprenant la réaction, dans un solvant organique inerte, d'un composé hétérocyclique tel que l'oxirane, l'aziridine, l'oxétane, ou l'azétidine, avec du peroxyde d'azote ou de l'anhydride azotique. Lorsque l'oxyde d'azote est le peroxyde d'azote, les substituants nitroso du produit obtenu sont transformés en substituants nitro. Les composés hétérocycliques peuvent être substitués ou non. Le solvant est avantageusement un alcane chloré. Le procédé permet la réalisation de nouveaux dérivés nitratés du polybutadiène qui sont des caoutchoucs liquides lorsque la matière première a une masse moléculaire comprise entre 2000 et 10 000. Application à la fabrication de matériaux riches en énergie. The invention relates to the manufacture of energy-rich materials. It relates to a process comprising the reaction, in an inert organic solvent, of a heterocyclic compound such as oxirane, aziridine, oxetane, or azetidine, with nitrogen peroxide or nitrogen anhydride. When the nitrogen oxide is nitrogen peroxide, the nitroso substituents of the product obtained are converted into nitro substituents. The heterocyclic compounds may or may not be substituted. The solvent is advantageously a chlorinated alkane. The process allows the production of new nitrate derivatives of polybutadiene which are liquid rubbers when the raw material has a molecular mass of between 2000 and 10,000. Application to the manufacture of materials rich in energy.

Siphon-like process for the heavy part of a mixture of immiscible liquids in a sedimentation vessel and process for its operation

Process for preparing nitrooxyderivatives of naproxen

The present invention refers to a process for preparing a compound of general formula (A), as reported in the description, wherein R is a radical of naproxen or bromonaproxen and R 1 –R 12 are hydrogen or alkyl groups, m, n, o, q, r and s are each independently an integer from 0 to 6, and p is 0 or 1, and and X is O, S, SO, SO 2 , NR 13 or PR13 or an aryl, heteroaryl group, said process comprising reacting a compound of formula (B) R—COOZ  (B) wherein R is as defined above and Z is hydrogen or a cation selected from: Li+, Na+, K+, Ca++, Mg++, tetralkylammonium, tetralkylphosphonium, with a compound of formula (C), as reported in the description, wherein R1–R12 and m, n, o, p, q, r, s are as defined above and Y is a suitable leaving group.

Process for the production of esters of nitric acid

Apparatus for washing liquid and/or finely divided solid substances, such as nitrated products

731,014. Purifying liquids; gravity-separation apparatus. NITROGLYCERIN AKTIEBOLAGET. April 28, 1953 [April 29, 1952], No. 11664/53. Class 46. The apparatus shown is for washing a liquid such as a nitrated product with another liquid immiscible with it and having a different specific gravity. Washing liquid, such as water, to which an alkali has been added, introduced at 5, and nitroglycerine introduced at 4 are mixed in an injector 3 with the help of compressed air introduced at 6. The mixture passes into a chamber 1 where the air maintains vigorous movement before discharge at 9. The liquid mixture passes between plates 7 forming an angle of between 45 degrees and 60 degrees with the horizontal and spaced apart by a distance small (e.g. 5 mm.) compared with their extent into an intermediate compartment 8 and thence through openings 12 in a wall 10 into a separating chamber 11. From the latter the washing liquid overflows at 16 and the nitroglycerine at 15. The lower end of the separating chamber 11 communicates with an inspection glass 13 ; a layer h e of mixed liquids separating the two liquids may be maintained at the level of this glass by adjusting the height H between the overflow levels 15 and 16, for example with interchangeable nozzles.

PROCESS FOR THE PREPARATION OF MONONITROCHLOROBENZENE

DANS UN PROCEDE DE PREPARATION DU MONONITROCHLOROBENZENE PAR NITRATION DU CHLOROBENZENE UTILISANT UN MELANGE D'ACIDE NITRIQUE ET D'ACIDE PHOSPHORIQUE, LA REACTION DE NITRATION EST EFFECTUEE EN UTILISANT UN RAPPORT MOLAIRE ACIDE NITRIQUECHLOROBENZENE INFERIEUR OU EGAL A 1 EN PRESENCE D'ACIDE PHOSPHORIQUE CONCENTRE, A DES TEMPERATURES DE 50-120C EN MAINTENANT LA CONCENTRATION DE L'ACIDE PHOSPHORIQUE, EXPRIMEE EN PO, A 72,4 EN POIDS OU PLUS DURANT LA REACTION. IN A PROCESS FOR THE PREPARATION OF MONONITROCHLOROBENZENE BY NITRATION OF CHLOROBENZENE USING A MIXTURE OF NITRIC ACID AND PHOSPHORIC ACID, THE NITRATION REACTION IS PERFORMED BY USING A MOLAR RATIO OF NITRIC ACID CHLOROBENZENE CONCENTRATE IN PRESENT PHOSURIA OR EGPHOROBENZENE CONCENTRATED IN 1 PRESENT PHOSURIA OR PHOSPHORIC ACID. AT TEMPERATURES OF 50-120C MAINTAINING THE CONCENTRATION OF PHOSPHORIC ACID, EXPRESSED IN PO, AT 72.4 BY WEIGHT OR MORE DURING THE REACTION.

Quinone based nitric oxide donating compounds

The present invention relates to nitric oxide donor compounds having a quinone based structure of formula (I), wherein R1 to R6, m, n and p are as defined in claim 1, to processes for their preparation and to their use in the treatment of pathological conditions where a deficit of NO plays an important role in their pathogenesis, such as pulmonary arterial hypertension, Sickle cell disease, systemic sclerosis and scleroderma, muscular dystrophies, Duchenne's muscular dystrophy and Becker's muscular dystrophy, vascular dysfunctions.

Alpha-substituted glycerol nitrates

Process for preparing halogenoalkzlnitrates

Rastvor koji sadrži:a) jedinjenje prema opštoj formuli (I)X-(CH2)n-ONO2 (I)gde je:X atom halogena odabran iz grupe koja se sastoji od Cl i Br, n je ceo broj od 3 do 6; ib) rastvarač izabran iz grupe koja se sastoji od CH2Cl2, CHCl3, CCl4, perfluorheksana, perfluorheptana;naznačen time što je jedinjenje prema formuli (I) prisutno u koncentraciji koja nije viša od 20%, u odnosu na masu.Prijava sadrži još 7 patentnih zahteva.

Process for the preparation of naproxene nitroxyalkylesters

A process for obtaining nitroxyalkylesters of the 2-(S)-(6-methoxy-2-naphthyl)-propanoic acid having an enantiomeric excess higher than or equal to 95 %, preferably higher than or equal to 98 %, characterized in that an halide of the 2-(S)-(6-methoxy-2-naphthyl)-propanoic acid of formula A-Hal, wherein A is the acid acyl residue, is reacted in an inert organic solvent with an aliphatic nitroxyalkanol HO-Y-ONO2, wherein Y is a C2-C20 alkylene or a cycloalkylene from 3 to 8 carbon atoms, or an alkylene as defined containing a cycloalkylene as defined, in the presence of an inorganic base.

Production of fatty olefin derivatives via olefin metathesis (divisional application 201801337)

EN UN ASPECTO, LA INVENCIÓN PROPORCIONA UN MÉTODO PARA LA SÍNTESIS DE UN DERIVADO DE OLEFINA GRASA. EL MÉTODO INCLUYE: A) EL CONTACTO DE UNA OLEFINA DE ACUERDO CON LA FÓRMULA I (I), CON UN COMPAÑERO DE REACCIÓN DE METÁTESIS DE ACUERDO CON LA FÓRMULA IIB (IIB), EN PRESENCIA DE UN CATALIZADOR DE METÁTESIS EN CONDICIONES SUFICIENTES PARA FORMAR UN PRODUCTO DE METÁTESIS DE ACUERDO CON LA FÓRMULA IIIB: (IIIB); Y B) LA CONVERSIÓN DEL PRODUCTO DE METÁTESIS AL DERIVADO DE OLEFINA GRASA. CADA R1 SE SELECCIONA DE MANERA INDEPENDIENTE DE H, C1–18 ALQUILO Y C2–18 ALQUENILO; R2B ES C1–8 ALQUILO; SUBÍNDICE Y ES UN NÚMERO ENTERO QUE VARÍA DE 0 A 17; Y EL SUBÍNDICE Z ES UN NÚMERO ENTERO QUE VARÍA DE 0 A 17. EN CIERTAS FORMAS DE REALIZACIÓN, EL CATALIZADOR DE METÁTESIS ES UN CATALIZADOR DE TUNGSTENO O UN CATALIZADOR DE MOLIBDENO. EN DIVERSAS FORMAS DE REALIZACIÓN, EL DERIVADO DE OLEFINA GRASA ES UNA FEROMONA DE INSECTO. SE DESCRIBEN ADEMÁS COMPOSICIONES DE FEROMONAS Y MÉTODOS PARA SU USO. IN ONE ASPECT, THE INVENTION PROVIDES A METHOD FOR THE SYNTHESIS OF A OLEFIN FATTY DERIVATIVE. THE METHOD INCLUDES: A) CONTACT OF AN OLEFIN ACCORDING TO FORMULA I (I), WITH A METATHESIS REACTION PARTNER ACCORDING TO FORMULA IIB (IIB), IN THE PRESENCE OF A METATHESIS CATALYST UNDER CONDITIONS FOR FORMULA A METATHESIS PRODUCT IN ACCORDANCE WITH FORMULA IIIB: (IIIB); AND B) THE CONVERSION OF THE PRODUCT OF METATHESIS TO THE DERIVATIVE OF OLEFIN FAT. EACH R1 IS SELECTED INDEPENDENTLY FROM H, C1–18 ALKYL AND C2–18 ALKENYL; R2B IS C1–8 ALKYL; SUB-INDEX Y IS AN INTEGRAL NUMBER VARING FROM 0 TO 17; AND THE Z SUB-INDEX IS AN INTEGRAL NUMBER VARING FROM 0 TO 17. IN CERTAIN FORMS OF REALIZATION, THE METATHESIS CATALYST IS A TUNGSTENE CATALYST OR A MOLYBDENUM CATALYST. IN VARIOUS FORMS OF REALIZATION, THE OLEFIN FATTY DERIVATIVE IS AN INSECT PHEROMONE. COMPOSITIONS OF PHEROMONES AND METHODS FOR THEIR USE ARE ALSO DESCRIBED.

Centrifugal separator

Centrifugal separating device for liquids, having in combination a receptacle mounted to rotate about its vertical axis, means for rotating the receptacle, and collecting means for the separated liquid components, said receptacle comprising a receiving chamber on top therein for the reception of the liquid feed, a plurality of spaced passages extending downward and outwardly through the wall of the receptacle from a point adjacent to the intersection of the bottom and the wall of the receiving chamber, a separation chamber located below the receiving chamber and in communication with the receiving chamber by means of said steps, an obstacle disposed at the bottom of the wall of the separating chamber and extending substantially horizontally inwardly and then substantially vertically downwards, an outlet ring for the heavier liquid component, which leads outward from e the surface of the obstacle at points adjacent to the intersection of the wall of the separating chamber and the horizontal surface of the obstacle and a plurality of spaced outlet ducts for the lighter liquid component leading outward from the vertical surface of the obstacle in points adjacent to the bottom of the separating chamber, said outlet ring and exit conduits for the liquid components being in communication with said collecting means. (Machine-translation by Google Translate, not legally binding)

Process of nitration

Nitrate esters of hydroxy carboxylic acids and the preparation thereof

The invention comprises nitrates of the formula <FORM:1078045/C2/1> wherein R1 is C4- 12 straight chain alkyl and X is hydrogen or straight-chain alkyl group and a more general method of preparation of compounds of the formula <FORM:1078045/C2/2> where R is a straight chain alkyl group of at least 3 carbon atoms comprising introducing a mixture of one or more straight chain a -olefins, having at least 5 carbon atoms, and molecular oxygen into liquid dinitrogen tetroxide at - 10 DEG to +40 DEG C., removing excess nitrous fumes at a temperature not exceeding 60 DEG C. and, if desired, esterifying the carboxyl group in a known manner. The oxygen and dinitrogen tetraoxide are used in at least equimolar amounts, based on olefin. The reaction may be effected in the presence of an oxidation catalyst, e.g. SeO2 or V2O5. The starting olefin may be used in the form of a commercial mixture containing saturated hydrocarbons which act as a diluent. The excess nitrous fumes are conveniently removed from the product using a thin film evaporator. Examples relate to the nitrate esters of methyl-a -hydroxyvalerate, methyl - a - hydroxyoenanthate, a -hydroxycaprylic acid, a -hydroxycapric acid, a -hydroxylauric acid, a -hydroxymyristic acid, a -hydroxypelargonic acid, a -hydroxystearic acid, a -hydroxyarachidic acid and a -hydroxy-nonadecane carboxylic acid.

Process for preparing nitrooxy esters, nitrooxy thioesters, nitrooxy carbonates and nitrooxy thiocarbonates, intermediates useful in said process and preparation thereof

The present invention relates to a process for preparing nitrooxy esters, nitrooxy thioesters, nitrooxy carbonates and nitrooxy thiocarbonates of compounds having at least a hydroxyl or thiol functional group, according to the following reaction scheme, (I), (II), (III). The invention also relates to intermediates useful in said process and to their preparation.

A kind of production method of isooctyl ester nitrate

本发明提供了一种硝酸异辛酯的生产方法，主要包括：通过可靠、稳定的进料设备计量输送硝硫混酸与异辛醇原料，两股原料在微混合器中混合与反应，混合后的物料在微换热器中经热交换，进入单管反应器中进一步反应，反应产物在自动分离器中分离出酸性硝酸异辛酯和废酸，酸性硝酸异辛酯迅速在一系列微混合器中经常规的水洗、碱洗再水洗过程，最后经干燥或静置除去其中的水分即得产品硝酸异辛酯。本发明方法硝化过程安全高效，原料异辛醇转化率和产品选择性皆高于99.5％，产品酸度值可达到0。

Device for producing methyl formate by gas phase methanol carbonylation, process and catalyst on-line evaluation method

本发明公开了一种气相甲醇羰基化生产甲酸甲酯的装置，其特征在于：该装置包括氮气气体管道、一氧化碳气体管道、氢气气体管道、一氧化氮气体管道、氧气气体管道、甲醇储罐(1)、流体泵(2)、酯化塔(3)、第一精馏塔(4)、废水储罐(5)、第一冷凝器(6)、气体混合箱(7)、反应器(8)、加热炉(9)、催化剂(10)、针型阀(11)、在线气相色谱分析系统(12)、气液分离器(13)、第二精馏塔(14)、第二冷凝器(15)、甲酸甲酯储罐(16)、放空阀(17)、循环泵(18)。该装置采用固定床反应器，催化剂与产物易分离，装置操作简单，反应器为常压反应器，资金投入少。

Process for preparing halogenoalkylnitrates

A process for preparing a compound of formula (I) X-(CH2)n-ONO2 (I) wherein: X is a halogen atom selected from Cl, Br, I; n is an integer from 3 to 6; said process comprising the slow addition of a compound of formula (II) X-(CH2)n-OH (II) wherein X and n are as defined above to a nitrating agent selected from the group consisting of concentrated nitric acid/concentrated sulfuric acid (sulfonitric mixture), nitric acid alone, NaNO2 in trifluoroacetic acid, nitronium salts such as NO2BF4 and an organic solvent selected from the group consisting of CH2Cl2, CHCl3, CCl4, perfluorohexane, perfluoroheptane. The invention refers also to solutions containing: a compound of general formula (I) and a solvent selected from the group consisting of CH2Cl2, CHCl3, CCl4, perfluorohexane, perfluoroheptane, characterized in that the compound of formula (I) is present in a concentration not higher than 20% by weight.

A kind of method of acid and water in removing isooctyl ester nitrate

针对现有技术中除去硝酸异辛酯中酸和水的方法存在危险性高，投入成本大等缺陷，本发明提供一种除去硝酸异辛酯中酸和水的方法，包括以下步骤：(1)将混有酸和水的硝酸异辛酯混合物置于第一容器中，加入盐溶液；(2)静置，待分层后，分离成油相和水相。本发明是一种安全性能高、操作简易、成本低、效果好的除去硝酸异辛酯中酸和水的方法。

Manufacturing process of organic nitrates

Safe way to get vicinal glycol dinitrates

РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2017 138 019 A (51) МПК C07C 201/02 (2006.01) C07C 203/04 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ЗАЯВКА НА ИЗОБРЕТЕНИЕ (21) (22) Заявка: 2017138019, 31.10.2017 Приоритет(ы): (22) Дата подачи заявки: 31.10.2017 (43) Дата публикации заявки: 06.05.2019 Бюл. № 13 R U (57) Формула изобретения 1. Способ получения динитратов вицинальных гликолей, заключающийся в том, что исходные гликоли сульфатируют действием концентрированной серной кислоты с образованием кислых сульфатов с последующей их обработкой во второй стадии нитрующей смесью в присутствии хлорорганических растворителей. 2. Способ по п. 1, отличающийся тем, что сульфатирование проводят с получением смеси моно- и дисульфата гликоля. 3. Способ по п. 1, отличающийся тем, что и первую и вторую стадии проводят при температурах до 35°С без потери в выходе целевого продукта. 4. Способ по п. 1, отличающийся тем, что в качестве хлорорганического растворителя используют хлористый метилен. Стр.: 1 A 2 0 1 7 1 3 8 0 1 9 A (54) Безопасный способ получения динитратов вицинальных гликолей 2 0 1 7 1 3 8 0 1 9 (72) Автор(ы): Астратьев Александр Александрович (RU), Викентьева Юлия Артуровна (RU), Кузнецов Леонид Леонидович (RU), Сибирев Владимир Владимирович (RU), Скороходов Константин Валентинович (RU), Санников Владимир Сергеевич (RU) R U Адрес для переписки: 192076, Санкт-Петербург, Советский пр., 33А, ФГУП "СКТБ "Технолог" (71) Заявитель(и): Федеральное государственное унитарное предприятие "Специальное конструкторско-технологическое бюро "Технолог" (RU)

Co-nitrating

Zeigler Case 2 CO-NITRATING Abstract of the Invention It has been discovered that when co-nitrating a mixture of trimethylolethane and diethylene glycol, a storage stable spent acid can be obtained if during the co-nitration an excess of from about 60 to about 100% by weight of nitric acid over that stoichiometrically required is employed.

Nitrate ester preparation

The process of the present invention provides a method of obtaining a high yield of water or acid soluble nitrate esters without the use of organic solvents in the nitration reaction or the production of unstable products or by-products. The process involves the nitration of an organic hydroxy-containing compound with a suitable nitrating agent such as nitric acid in the absence of organic solvents in the nitration reaction. The reaction mixture is neutralized, causing the nitrate esters to precipitate or separate from the neutralized nitrate solution. The nitrate ester is then recovered, and any dissolved nitrate salts can be removed therefrom by gentle washing with water or a dilute halide solution. As provided by the process of the present invention, no organic solvents are used in the nitration reaction and average yields range from about 80% to about 95%.

PROCEDURE FOR THE NITRATION OF ALCANDIOLI.

A process for the preparation of compounds of formula HO-A-ONO2&emsp;&emsp;(I) wherein A is a C2-C6 alkylene chain by nitration of the corresponding alkanediols with &ldquo;stabilized&rdquo; nitric acid is herein disclosed. The process is safer to operators and allows to obtain advantageous yields on an industrial scale.

Process for preparing nitrooxyalkyl substituted esters of carboxylic acids, intermediates useful in said process and preparation thereof

The present invention refers to a process for preparing a compound of general formula (A), as reported in the description, wherein R is a radical of a drug and R1-R12 are hydrogen or alkyl groups, m, n, o, q, r and s are each independently an integer from 0 to 6, and p is 0 or 1, and X is O, S, SO, SO2, NR13 or PR13 or an aryl, heteroaryl group, said process comprising reacting a compound of formula (B) R-COOZ (B) wherein R is as defined above and Z is hydrogen or a cation selected from: Li+, Na+, K+, Ca++, Mg++, tetralkylammonium, tetralkylphosphonium, with a compound of formula (C), as reported in the description, wherein R1-R12 and m, n, o, p, q, r, s are as defined above and Y is a suitable leaving group.