Method for Preparing Crosslinker Compound

The present disclosure relates to a method for preparing a crosslinker compound in which a crosslinker compound capable of using for the production of a super absorbent polymer can be obtained in a higher yield by a simple manner. The crosslinker compound obtained by the above method can be used as a thermally decomposable crosslinker in the process of producing a super absorbent polymer.

METHODS FOR MAKING VALERENIC ACID DERIVATIVES AND THEIR USE

The present invention is directed to compounds, intermediates and methods for making valerenic acid and its derivatives as well as the use of such compounds as GABAreceptor ligands. 2. (canceled)7. A compound according to claim 1 , wherein the bond between Cand Cis a double bond.8. A compound according to claim 1 , wherein Ris H.9. A compound according to claim 1 , wherein Ris H.1014-. (canceled)15. A pharmaceutical composition comprising a pharmaceutically effective amount of a compound according to claim 1 , optionally in the form of an ester prodrug.1617-. (canceled) The present invention relates to valerenic acid derivatives being suitable for pharmaceutical compositions and methods for making them. Furthermore, the present invention relates to pharmaceutical compositions comprising said compounds, which exhibit GABAreceptor binding activity. Said compositions may particularly be used for the treatment of anxiety and insomnia.Insomnia and anxiety are two conditions, which have substantial negative impact on day-to-day quality of life. Insomnia is often described as subjective complaint of poor sleep quality or quantity despite adequate time for sleep. Insomnia results in daytime fatigue, irritability and decreased concentration and is often associated with other diseases such as psychiatric disorders (e.g. anxiety conditions), medical disorders or substance abuse. Anxiety also leads to fatigue, irritability and decreased concentration. Several forms of anxiety are known, such as generalized anxiety disorder, panic disorder, social anxiety disorder and post-traumatic stress disorder. Effective treatment of said conditions thus positively influences day-to-day life of patients suffering from such conditions.Current pharmaceuticals used for the treatment of insomnia and anxiety comprise benzodiazepines, benzodiazepine-receptor agonists, melatonin-receptor agonists as well as antidepressants. However, most of said drugs exhibit strong adverse effects such as ...

Hydrogenation and ethynylation catalysts

A process for preparing a catalyst includes impregnating a metal oxide carrier with an aqueous solution to form an impregnated carrier; drying the impregnated carrier to form a dried, impregnated carrier; and heat-treating the dried, impregnated carrier in air to form the catalyst; wherein: the aqueous solution includes a copper salt; and from about 3 wt % to about 15 wt % of a C3-C6 multifunctional carboxylic acid; and the catalyst includes from about 5 wt % to about 50 wt % copper oxide.

TREPROSTINIL PRODUCTION

The present invention is directed to a novel method for preparing a synthetic intermediates for treprostinil. Also described are methods of preparing treprostinil comprising utilizing novel intermediates described herein as well as novel intermediates useful for synthesis prostacyclin derivatives, such as treprostinil. 2. The process of including the additional claim 1 , final step of converting the treprostinil so formed to its sodium salt. The present application is a Continuation of U.S. application Ser. No. 13/435,708, filed Mar. 30, 2012, which is a Continuation of U.S. application Ser. No. 13/151,465, filed Jun. 2, 2011, which claims the benefit of U.S. provisional application No. 61/351,115 filed Jun. 3, 2010, which are incorporated herein by reference in their entirety.The present application relates to a process for producing prostacyclin derivatives, such as Treprostinil, and novel intermediate compounds useful in the process.(+)-Treprostinil (also known as UT-15) is the active ingredient in Remodulin®, a commercial drug approved by FDA for the treatment of pulmonary arterial hypertension (PAH). It was first described in U.S. Pat. No. 4,306,075. Treprostinil is a stable analog of prostacyclin (PGI) belonging to a class of compounds known as benzindene prostacyclins, which are useful pharmaceutical compounds possessing activities such as platelet aggregation inhibition, gastric secretion reduction, lesion inhibition, and bronchodilation.U.S. Pat. No. 5,153,222 describes use of treprostinil for treatment of pulmonary hypertension. Treprostinil is approved for the intravenous as well as subcutaneous route, the latter avoiding potential septic events associated with continuous intravenous catheters. U.S. Pat. Nos. 6,521,212 and 6,756,033 describe administration of treprostinil by inhalation for treatment of pulmonary hypertension, peripheral vascular disease and other diseases and conditions. U.S. Pat. No. 6,803,386 discloses administration of treprostinil for ...

Novel Ethynylation Catalyst And Method Of Making Same

A novel catalyst useful in the ethynylation of formaldehyde to butynediol is formed by precipitating copper and bismuth from a salt solution of such metals, utilizing an alkali metal hydroxide as the precipitating agent to deposit copper and bismuth hydroxide as a coating around a siliceous carrier particle. 1. A method of preparing a catalyst for the ethynylation of formaldehyde which comprises: depositing by precipitation copper hydroxide , over a particulate siliceous carrier and calcining the treated carrier to yield a copper oxide coating around the carrier.2. The method of claim 1 , wherein a mixture of copper and bismuth hydroxides are deposited on said carrier.3. The method of claim 1 , wherein the copper hydroxide is formed by adding an alkali metal hydroxide to an acidic copper salt solution.4. The method of claim 3 , wherein an acidic solution is made of a mixture of copper nitrate and bismuth nitrate.5. The method of claim 3 , wherein said alkali metal hydroxide is sodium hydroxide.6. The method of claim 5 , wherein the sodium hydroxide is provided in a separate vessel from the acidic solution claim 5 , and the siliceous carrier particles are provided in water in a precipitation vessel separate from the sodium hydroxide and acidic solution.7. The method of claim 6 , wherein the acidic solution and the sodium hydroxide are added simultaneously to the precipitation vessel.8. The method of claim 6 , wherein the precipitation is carried out at a constant pH of between about 6 to about 10.9. The method of claim 6 , wherein the precipitation is carried out at a contrast pH of between 7.5 to 9.5.10. The method of claim 6 , wherein the precipitation is carried out at a temperature of about 40° C. to 90° C.11. The method of claim 10 , wherein the temperature is between 45° C. to 65° C.12. The method of claim 1 , wherein the precipitate is filtered claim 1 , washed and dried and the dried material calcined in air at a temperature between about 250 to about 550° C. ...

CATALYTIC ETHYNYLATION

The present invention relates to the catalytic ethynlation of αβ-unsaturated ketones for producing tertiary acetylenic alcohols. 2. Process according to claim 1 , whereinR is an aliphatic or aromatic hydrocarbon which is substituted with lower alkoxy or lower alkyl groups and{'sub': 1', '3, 'Ris CH.'}4. Process according to claim 1 , wherein the process is carried out at a temperature below +5° C.5. Process according to claim 1 , wherein the process is carried out at a temperature of from −60° C. to 5° C.6. Process according to claim 1 , wherein the process is carried out at atmospheric conditions.7. Process according to claim 1 , wherein the process is carried out at elevated pressure.8. Process according to claim 1 , herein the process is carried without any addition of water. The present invention relates to the catalytic ethynylation of α,β-unsaturated ketones for producing tertiary acetylenic alcohols.The ethynyated reaction products, α-alkynols, are important intermediates in organic synthesis. For example, ethynyl-β-ionol is an intermediate used in the preparation of vitamin A and β-carotene.The process for ethynylating of α,β-unsaturated ketones for producing tertiary acetylenic alcohols is well known and described in many patent (i.e. in U.S. Pat. Nos. 3,709,946; 3,082,260, 3,283,014, 4,147,886 and 4,320,236).In U.S. Pat. No. 4,320,236, the ethynylation is carried out in the presence of a monolithium acetylide-ammonia complex.In U.S. Pat. No. 4,147,886, the ethynylation is carried out in the presence of diluted KOH.Due to the importance of the ethynylated reaction products, there is always a need for an improved way to producing such products.Surprisingly, it was found that the use of solid KOH in the reaction process allows to carry out the ethynylation process in an easy way.Therefore, the present invention relates to a process (P) to produce compounds of formula (III)whereinR is hydrogen or an aliphatic, cyclo-aliphatic or aromatic hydrocarbon which can ...

SPRAY-DRIED BUTYNEDIOL CATALYSTS

A process of forming an ethynylation catalyst includes providing a slurry including water, a copper-containing material, a bismuth-containing material, a structural material, and a binder; spray-drying the slurry to form particles; and calcining the particles to form the ethynylation catalyst. 1. A process of forming an ethynylation catalyst , the process comprising:providing an aqueous slurry comprising water, a copper-containing material, a bismuth-containing material, a structural material, and a binder;spray-drying the slurry to form particles; andcalcining the particles to form the ethynylation catalyst.2. The process of claim 1 , wherein the copper-containing material comprises copper carbonate claim 1 , copper oxalate claim 1 , copper hydroxide claim 1 , cupric oxide claim 1 , or cuprous oxide.3. The process of claim 1 , wherein the bismuth-containing material comprises bismuth carbonate claim 1 , bismuth oxalate claim 1 , bismuth hydroxide claim 1 , bismuth oxide claim 1 , and bismuth acetate.4. The process of claim 1 , wherein the structural material comprises a clay claim 1 , talc claim 1 , calcium silicate claim 1 , kieselguhr claim 1 , alumina claim 1 , carbon claim 1 , or silica.5. The process of claim 1 , wherein the binder comprises a silica sol claim 1 , an alumina sol claim 1 , sodium silicate claim 1 , or aluminum chlorohydrate.6. The process of claim 1 , wherein the particles have an average particle diameter of about 5 μm to about 100 μm.7. The process of claim 1 , wherein the particles have an average particle diameter of about 5 μm to about 60 μm.8. The process of claim 1 , wherein the particles have an average particle diameter of about 15 μm.9. The ethynylation catalyst formed according to .10. A process of activating an ethynylation catalyst claim 1 , the process comprising:{'claim-ref': {'@idref': 'CLM-00009', 'claim 9'}, 'providing the ethynylation catalyst of ;'}exposing the ethynylation catalyst to formaldehyde to form a mixture; ...

ETHYNYLATION OF POLYUNSATURATED ALDEHYDES AND KETONES

The present invention relates to a catalytic process for the ethynylation of specific polyunsaturated aldehydes and ketones. 5. The catalytic ethynylation process according to claim 1 , wherein the catalyst is added to the reaction mixture as an aqueous solution.6. The catalytic ethynylation process according to claim 1 , wherein R is K.7. The catalytic ethynylation process according to claim 1 , wherein the catalytic ethynylation reaction is carried out under pressure which is in a range from 2 bar to 15 bar.8. The catalytic ethynylation process according to claim 1 , wherein the catalytic ethynylation reaction temperature is between −30° to 5° C.9. The catalytic ethinylation process according to claim 1 , wherein the catalytic ethynylation reaction is carried out under pressure which is in a range of 5 bar to 12 bar.10. The catalytic ethinylation process according to claim 1 , wherein the catalytic ethynylation reaction is carried out under pressure which is in a range of 6 bar to 10 bar. This application is a continuation of commonly owned copending U.S. application Ser. No. 15/518,080, filed Apr. 10, 2017 (now abandoned), which is the U.S. national phase of International Application No. PCT/EP2015/073868 filed Oct. 15, 2015, which designated the U.S. and claims priority to EP Patent Application No. 14189262.0, filed Oct. 16, 2014, the entire contents of each of which are hereby incorporated by reference.The present invention relates to a catalytic process for the ethynylation of specific polyunsaturated aldehydes and ketones.Polyunsaturated aldehydes and ketones in the context of the present invention are aldehydes and ketones wherein the aldehydes and ketones comprise at least two C—C double bonds. In some embodiments of the present invention the C—C double bonds can also be conjugated.Polyunsaturated aldehydes and ketones (with conjugated C—C double bonds), such as the α,β-unsaturated ones, are quite stable compounds.The reaction products, which are the ...

NOVEL ETHYNYLATION CATALYST AND METHOD OF MAKING SAME

A novel catalyst useful in the ethynylation of formaldehyde to butynediol is formed by precipitating copper and bismuth from a salt solution of such metals, utilizing an alkali metal hydroxide as the precipitating agent to deposit copper and bismuth hydroxide as a coating around a siliceous carrier particle. 1. A method of preparing a catalyst for the ethynylation of formaldehyde which comprises: depositing by precipitation copper hydroxide via the reaction of an acidic copper salt solution with an alkaline metal hydroxide , on a particulate siliceous carrier , and calcining the treated carrier to yield a copper oxide coating around said particulate siliceous carrier.2. The method of claim 1 , wherein a mixture of copper and bismuth hydroxides are deposited on said carrier.3. (canceled)4. The method of claim 1 , wherein said acidic solution is made of a mixture of copper nitrate and bismuth nitrate.5. The method of claim 1 , wherein said alkali metal hydroxide is sodium hydroxide.6. The method of claim 5 , wherein the sodium hydroxide is provided in a separate vessel from the acidic solution claim 5 , and the siliceous carrier particles are provided in water in a precipitation vessel separate from the sodium hydroxide and acidic solution.7. The method of claim 5 , wherein said acidic solution and said sodium hydroxide are added simultaneously to the precipitation vessel.8. The method of claim 6 , wherein said precipitation is carried out at a constant pH of between about 6 to about 10.9. The method of claim 6 , wherein said precipitation is carried out at a contrast pH of between 7.5 to 9.5.10. The method of claim 6 , wherein said precipitation is carried out at a temperature of about 40° C. to 90° C.11. The method of claim 10 , wherein said temperature is between 45° C. to 65° C.12. The method of claim 1 , wherein said precipitate is filtered claim 1 , washed and dried and the dried material calcined in air at a temperature between about 250 to about 550° C.13. The ...

METHODS OF PRODUCING DICARBONYL COMPOUNDS

Dicarboxylic acids, such as adipic acid, and diesters, such as adipates, may be produced by hydrogenating alkynes that may be produced from raw materials salvaged from waste stream processes. The carbons of the dicarboxylic acids are provided by alkynes generated from biomass waste and carbon dioxide recovered from waste streams such as exhaust gases. 2. The method of claim 1 , wherein n is less than or equal to about 20.3. The method of claim 1 , wherein the hydrogenating comprises a catalytic hydrogenation.56.-. (canceled)7. The method of claim 4 , further comprising preparing the alkyne of formula III by base promoted elimination of hydrogen halide from a dihalo-alkyne of formula IV:{'br': None, 'sub': n', '(2n-4z), 'X—(CH—X (IV),'}whereinz is a number of (—C≡C—) moieties,z=m-1, andeach X comprises a same or different one of F, Cl, Br, I, and At.1013.-. (canceled)14. The method of claim 1 , wherein R=H claim 1 , n=4 claim 1 , m=2 claim 1 , and the bis-carbonyl alkyne is a bis-carboxy alkyne of a formula HOOC—C≡C—C≡C—COOH.15. The method of claim 14 , further comprising producing the bis-carboxy alkyne of formula HOOC—C≡C—C≡C—COOH by carboxylating diacetylene with COin the presence of a first metal catalyst including copper claim 14 , silver claim 14 , bismuth or combinations thereof.16. (canceled)17. The method of claim 15 , further comprising producing the diacetylene by base promoted elimination of HCl from 1 claim 15 ,4-dihalo-2-butyne.18. The method of claim 17 , further comprising producing the 1 claim 17 ,4-dihalo-2-butyne by treating 2-butyne-1 claim 17 ,4-diol with thionyl chloride.19. (canceled)20. The method of claim 18 , further comprising producing the 2-butyne-1 claim 18 ,4-diol by contacting acetylene and formaldehyde in the presence of a second metal catalyst including copper claim 18 , silver claim 18 , bismuth or combinations thereof.2122.-. (canceled)23. The method of claim 20 , further comprising producing the acetylene by pyrolysis of ...

(6R,10R)-6,10,14-TRIMETYLPENTADECAN-2-ONE PREPARED FROM 6,10,14 TRIMETYLPENTADECA-5,9,13-TRIEN-2-ONE OR 6,10,14-TRIMETYLPENTADECA-5,9-DIEN-2-ONE

The present invention relates to a process of manufacturing (6R,10R)-6,10,14-trimethylpentadecan-2-one in a multistep synthesis from a mixture of (5E,9E)-, (5E,9Z)-, (5Z,9E)- and (5Z.9Z)-isomers of 6,10,14-trimethylpentadeca-5,9,13-trien-2-one or 6,10,14-trimethylpentadeca-5,9-dien-2-one. The process is very advantageous in that it forms in an efficient way the desired chiral product from a mixture of stereoisomers of the starting product.

PROCESS FOR THE PRODUCTION OF 2-ALKYL-3-BUTYN-2-OLS

The present invention relates to an improved process for the production of 2-alkyl-3-butin-2-ols; especially to a new purification step. 2. Process according to claim 1 , wherein R is —CH.3. Process according to claim 1 , wherein the extraction solvent is MTBE and/or ETBE claim 1 , preferably MTBE.4. Process according to claim 1 , wherein the alkali metal hydroxide catalyst in step i) is KOH or NaOH claim 1 , preferably KOH.5. Process according to claim 1 , wherein in step iiia) the alkali metal hydroxide is NaOH and/or KOH claim 1 , preferably it is KOH.6. Process according to claim 1 , wherein step iiia) is carried out at temperature of 10-45° C. claim 1 , preferably 20-30° C.7. Process according to claim 1 , wherein the alkali metal hydroxide catalyst in step i) is present in catalytic amounts.8. Process according to claim 1 , wherein alkali metal hydroxide in step iiia) can further be added during step iv).9. Process according to claim 1 , wherein step iiia) is carried out at normal pressure (1 bar). The present invention relates to an improved process for the production of 2-alkyl-3-butin-2-ols; especially to a new purification step.The 2-alkyl-3-butin-2-ols, which are produced by the process according to the present invention are 2-ethyl-3-butin-2-ol (EBI) and 2-methyl-3-butin-2-ol (MBI).EBI and MBI are very well-known and versatile products in the chemical industry. They are used for example in the process of production of isoprenes, vitamin A, vitamin E as well as for the production of fragrance and flavour compounds.Due to the various uses of EBI and MBI, it is important and crucial to have an easy and effective way to produce EBI and MBI in an industrial scale.Usually EBI is produced by the reaction of butan-2-one (methylacetone) and ethyne (acetylene) in the presence of liquid ammonia as a solvent and an alkali metal hydroxide andMBI is produced by the reaction of propan-2-one (acetone) and ethyne (acetylene) in the presence of liquid ammonia as a solvent ...

Alkenes as alkyne equivalents in radical cascades terminated by fragmentations

Disclosed are methods for rerouting radical cascade cyclizations by using alkenes as alkyne equivalents. The reaction sequence is initiated by a novel 1,2 stannyl shift which achieves chemo- and regioselectivity in the process. The radical “hopping” leads to the formation of the radical center necessary for the sequence of selective cyclizations and fragmentations to follow. In the last step of the cascade, the elimination of a rationally designed radical leaving group via β-C—C bond scission aromatizes the product without the need for external oxidant. The Bu 3 Sn moiety, which is installed during the reaction sequence, allows further functionalization of the product via facile reactions with electrophiles as well as Stille and Suzuki cross-coupling reactions. This selective radical transformation opens a new approach for the controlled transformation of enynes into extended polycyclic structures of tunable dimensions.

Production of butanediol from a methane conversion process

Methods and systems are provided for converting methane in a feed stream to butanediol. The method includes processing acetylene as an intermediate stream to form a hydrocarbon stream including butanediol. A hydrocarbon stream is introduced into a supersonic reactor and pyrolyzed to convert at least a portion of the methane to acetylene. The reactor effluent stream is treated to convert acetylene to another hydrocarbon process. The method according to certain aspects includes controlling the level of carbon monoxide to prevent undesired reactions in downstream processing units.

一种乙炔与甲醛制备1,4-丁二醇的强化系统及工艺

本发明适用于丁二醇的生产技术领域，提供了一种乙炔与甲醛制备1,4‑丁二醇的强化系统及工艺，包括依次对应连接的甲醛制备装置、1,4‑丁炔二醇制备装置、1,4‑丁二醇制备装置和精馏装置，还包括智能控制装置；1,4‑丁二醇制备装置包括1,4‑丁二醇反应器，其内部设有微界面发生器，微界面发生器将氢气破碎成直径≥1μm、且＜1mm的微米级气泡；入口端分别连接给料泵、催化剂进料结构和氢气罐，出口端连接催化剂回收器；智能控制装置包括策略设置单元、参数控制单元和模型设置单元。借此，本发明能够使加氢工段反应更充分，1,4‑丁二醇的产量更高，避免催化剂原料浪费，降低生产成本，实现智能化操作。

Ethynylation process

制备1,4-丁炔二醇催化剂的方法

本发明公开一种制备1,4-丁炔二醇催化剂的方法，包括如下步骤：（1）配制铜硅混合溶液、铜铋混合溶液、沉淀剂溶液Ⅰ和沉淀剂溶液Ⅱ；（2）往反应釜中加入底水，升温加热至反应温度；并流滴加共沉淀；（3）将物料经过过滤、洗涤，干燥后，过筛；收集过筛产物并将其加入反应釜中；（4）向步骤（3）中的反应釜加入底水，将铜铋混合溶液和沉淀剂溶液Ⅱ并流滴加共沉淀；（5）将物料过滤，洗涤后按固含量10%~40%，加入适量蒸馏水；（6）浆液采用喷雾干燥，干燥、焙烧得到生产1,4-丁炔二醇的催化剂。该催化剂具有耐磨性好、催化剂颗粒均匀、使用过程中不易流失、制备方法简单、易行、重复性好等优点。

Byd反应和催化剂分离再生方法及装置

本发明涉及1,4丁炔二醇反应和催化剂再生技术领域，是一种BYD反应和催化剂分离再生方法及装置，后者包括催化剂制备单元、催化剂活化单元、反应单元、催化剂沉降分离单元和催化剂洗涤再生单元。本发明结合BYD反应和催化剂分离再生方法及装置，在生产BYD的同时，催化剂采取外部沉降分离形式，避免产生大量的聚合物包裹催化剂表面，催化剂活性稳定，装置反应平稳，副产物大幅降低，实现高活性催化的再利用；本发明对反应器进行改进，取消了烛式过滤器，使得反应器内气、液、固三相接触更加充分；本发明装置相增设小型催化剂活化反应器，定期活化催化剂，使活化量大幅降低，活化后的催化剂采取定时定量补加入反应器。

Production of alkinols

Process

Spray-dried butynediol catalyst

A kind of bulky grain copper bismuth catalyst and its preparation method and application

本发明公开一种大颗粒铜铋催化剂的制备方法，包括以下步骤：（1）配制含有铜盐和铋盐的酸性溶液；（2）配制沉淀剂溶液；（3）往反应釜中加入底水，升温加热至反应温度；（4）采取并流的方式，将步骤（1）的酸性溶液和步骤（2）的沉淀剂溶液滴加到反应釜中；（5）当剩余酸性溶液为步骤（1）配制酸性溶液总量的4/5~9/10时，停止反应，进行老化；（6）老化结束后，继续进行反应并从反应釜底部继续通入气体CO 2 ；（7）当剩余酸性溶液为步骤（1）配制酸性溶液总量的1/5‑1/10时，提高向反应体系加水的流量；（8）待反应结束后，进行老化，老化结束后，洗涤，过滤。该方法制备的催化剂具有耐磨性好，催化剂颗粒大小均匀适中、活性稳定性高，丙炔醇的产量高等优点。

Patent HU166769B

METHOD OF ETHILATION

ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß (19) RU (11) 2005 107 412 (13) A (51) ÌÏÊ C07C 29/42 (2006.01) ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÇÀßÂÊÀ ÍÀ ÈÇÎÁÐÅÒÅÍÈÅ (21), (22) Çà âêà: 2005107412/04, 09.08.2003 (71) Çà âèòåëü(è): ÄÑÌ ÈÏ ÀÑÑÅÒÑ Á.Â. (NL) (30) Ïðèîðèòåò: 16.08.2002 EP 02018458.6 (43) Äàòà ïóáëèêàöèè çà âêè: 27.01.2006 Áþë. ¹ 03 (86) Çà âêà PCT: EP 03/08867 (09.08.2003) (87) Ïóáëèêàöè PCT: WO 2004/018400 (04.03.2004) Àäðåñ äë ïåðåïèñêè: 101000, Ìîñêâà, Ì.Çëàòîóñòèíñêèé ïåð., 10, êâ.15, "ÅÂÐÎÌÀÐÊÏÀÒ", È.À.Âåñåëèöêîé R U Ôîðìóëà èçîáðåòåíè 1. Ñïîñîá ïîëó÷åíè àöåòèëåíîâîíåíàñûùåííîãî ñïèðòà ðåàêöèåé êàðáîíèëüíîãî ñîåäèíåíè ñ àöåòèëåíîì â ïðèñóòñòâèè àììèàêà è ãèäðîêñèäà ùåëî÷íîãî ìåòàëëà, îòëè÷àþùèéñ òåì, ÷òî êàðáîíèëüíîå ñîåäèíåíèå ïðåäñòàâë åò ñîáîé ìåòèëýòèëêåòîí, ìåòèëãëèîêñàëüäèìåòèëàöåòàëü, 6-ìåòèë-5-ãåïòåí-2-îí, 6-ìåòèë-5-îêòåí-2-îí, ãåêñàãèäðîïñåâäîèîíîí, 4-(2,6,6-òðèìåòèë-1-öèêëîãåêñåí-1-èë)-3-áóòåí-2-îí èëè 6,10,14òðèìåòèë-2-ïåíòàäåêàíîí, ãèäðîêñèä ùåëî÷íîãî ìåòàëëà èñïîëüçóþò â âîäíîì ðàñòâîðå è ìîë ðíîå ñîîòíîøåíèå ìåæäó ýòèì ãèäðîêñèäîì ùåëî÷íîãî ìåòàëëà è êàðáîíèëüíûì ñîåäèíåíèå ñîñòàâë åò ìåíüøå 1:200. 2. Ñïîñîá ïî ï.1, â êîòîðîì ìîë ðíîå ñîîòíîøåíèå ìåæäó ãèäðîêñèäîì ùåëî÷íîãî ìåòàëëà è êàðáîíèëüíûì ñîåäèíåíèåì ñîñòàâë åò îò ïðèìåðíî 1:500 äî 1:200. 3. Ñïîñîá ïî ï.1, â êîòîðîì ìîë ðíîå ñîîòíîøåíèå ìåæäó ãèäðîêñèäîì ùåëî÷íîãî ìåòàëëà è êàðáîíèëüíûì ñîåäèíåíèåì ñîñòàâë åò îò ïðèìåðíî 1:300 äî ïðèìåðíî 1:220. 4. Ñïîñîá ïî ï.1, â êîòîðîì êàðáîíèëüíîå ñîåäèíåíèå ïðåäñòàâë åò ñîáîé 6-ìåòèë-5ãåïòåí-2-îí, à ïðîäóêòîì âë åòñ äåãèäðîëèíàëîîë. 5. Ñïîñîá ïî ï.1, â êîòîðîì ãèäðîêñèä ùåëî÷íîãî ìåòàëëà ïðåäñòàâë åò ñîáîé ãèäðîêñèä êàëè . 6. Ñïîñîá ïî ï.1, â êîòîðîì ðåàêöèþ ïðîâîä ò ïðè òåìïåðàòóðå îò ïðèìåðíî 0 äî ïðèìåðíî 40°Ñ, à äàâëåíèå äë óäåðæàíè àììèàêà â ñæèæåííîì ñîñòî íèè ðàâíî ñîîòâåòñòâóþùåìó çíà÷åíèþ, çàâèñ ùåìó îò ðåàêöèîííîé òåìïåðàòóðû, îò ïðèìåðíî 5 äî ïðèìåðíî 20 áàð (îò ïðèìåðíî 0,5 äî ïðèìåðíî 2 ÌÏà). 7. ...

Method for preparing alkyne diols possibly comprising alkyne monoalcohols

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to method for preparing alkyne diols possibly comprising alkyne mono- alcohols. Method involves interaction of ketones with acetylene hydrocarbons on organic solvent medium in the presence of a base followed by hydrolysis and isolation of the end substance. Acetylene hydrocarbons are taken among acetylene and alkyne aminoalcohols. Potassium alcoholates of primary and/or secondary alcohols or potassium alcoholates of primary and/or secondary alcohols containing KOH are used as a base. In using acetylene as an acetylene hydrocarbon the ratio of used ketone to acetylene is from 1.9:1 to 2.1:1 and the ratio of potassium alcoholate to used ketone is from 0.9:1 to 2.1: 1; in using alkyne monoalcohols as acetylene hydrocarbons the ratio of used alkyne monoalcohol to used ketone is from 1:0.8 to 1:1.2 and the ratio of potassium alcoholate to used ketone is from 1.5:1 to 2.2:1 to yield precipitating gel-like adducts of alkyne diols and, possibly, alkyne monoalcohol and a base. As result, the reaction mass retains capacity for stirring for all reaction time followed by hydrolysis of components. Method provides reducing amount of used solvent and provides preparing substances with improved indices for the further using. EFFECT: simplified and improved preparing method. 8 cl, 10 ex зЗэ9Эдгссс ПЧ сэ содержащих ацетиленовыми органическом растворителе в присутствии основания с последующим гидролизом и ацетиленового (19) РОССИЙСКОЕ АГЕНТСТВО ПО ПАТЕНТАМ И ТОВАРНЫМ ЗНАКАМ ВИ "” 2 221 768. (51) МПК? 13) С2 С 07С 33/044, 29/42 12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ РОССИЙСКОЙ ФЕДЕРАЦИИ (21), (22) Заявка: 2001107596/04, 13.08.1999 (24) Дата начала действия патента: 13.08.1999 (30) Приоритет: 17.08.1998 ОЕ 19837211.6 (46) Дата публикации: 20.01.2004 (56) Ссылки: СВ 1354011 А, 22.05.1974. СВ 1329815 А, 12.09.1973. СВ 1264194 А, 16.02.1972. ЗИ 318293 А, 30.08.1979. ЗЦ 639849 А, 30.12.1978. Щелкунов А.В. и др. ...

A kind of reactor and reaction system of synthesizing methyl butynol

本发明公开了一种合成甲基丁炔醇的反应器和反应系统，所述反应器包括依次连接的一段管式反应器和二段管式反应器，其中，所述一段管式反应器和二段管式反应器均包括管式反应器和设置在所述管式反应器内部的静态混合器。所述反应系统包括通过管路顺次连接的搅拌反应釜、反应器和终止混合器，其中，所述反应器采用上述合成甲基丁炔醇的反应器，所述搅拌反应釜的出料口与一段管式反应器的进料口连接并且所述二段管式反应器的出料口与终止混合器的进料口连接。本发明的合成甲基丁炔醇的反应器和反应系统不仅大大缩短了反应器的管程长度，而且也实现了物料的有效混合，避免了副反应的发生，与早期工艺相比大幅度提高了产品的收率。

Treprostinil prepatation

本发明公开了一种使用手性诱导剂通过立体选择性炔加成反应来制备用于曲前列环素的合成中间体的方法。本发明还描述了曲前列环素及其药学上可接受的盐的制备方法以及用于合成环前列腺素衍生物的新型中间体，所述制备方法包括所述炔加成反应。功能性醇保护基保护醇基使其不参与该分子的其他部分中发生的反应。所述中间体随后在转化之前被去保护且进行水解以获得最终的曲前列环素产物。

Process for preparing 6 -methyl -3 -heptene -2 -one and 6 -methyl -2 -heptane-one likes and process for preparing phytone or isophytol

本发明提供了通过在丙酮中各连续加入异戊醛和含有碱性物质的含水碱过程中进行的交叉醛醇缩合反应制备6－甲基－3－庚烯－2－酮的方法;制备由如上式(1)表示的6－甲基－2－庚烷酮类似物的方法,其中n是0或1或更大的整数;其方法包括使氢、丙酮和如上式(2)表示的醛在含有碱性物质的含水碱和氢化催化剂存在下反应,其中n如上定义;X和Y分别表示氢原子或它们连接在一起形成碳－碳键;和Z和W分别表示氢原子或它们连接在一起形成碳－碳键;和用6－甲基－3－庚烯－2－酮或6－甲基－2－庚烷酮类似物制备植酮或异植醇的方法。

Method for separation and recovery of propargyl alcohol

公开了分离并回收炔丙醇的方法，其特征在于使低聚甲醛和乙炔在催化剂的存在下于极性溶剂中反应得到的含有炔丙醇的产物混合物在100至150mmHg的压力下蒸馏。本方法不存在常规技术中存在的问题，允许以简单操作和有利的热量和能量分离和回收炔丙醇，而在含有溶剂、水和炔丙醇的产物混合物中分离回收炔丙醇时，不使用大型蒸馏装置复杂的方法或分离操作。

Specific α, the method for β unsaturated aldehydes are produced by rearrangement process

本发明涉及改进的生产特定α，β‑不饱和醛的方法。

An efficient process to induce enantioselectivity in procarbonyl compounds

Prepration method of cross-linking compound

본 발명은 고흡수성 수지의 제조를 위해 사용 가능한 가교제 화합물을 간단한 방법으로, 보다 높은 수율로 얻을 수 있는 가교제 화합물의 제조 방법에 관한 것이다. 이러한 방법으로 얻어진 가교제 화합물은 고흡수성 수지의 제조 과정에서, 열 분해 가능한 내부 가교제로서 바람직하게 사용될 수 있다. The present invention relates to a method for preparing a cross-linking agent compound that can be used for the production of a super absorbent polymer by a simple method and in a higher yield. The cross-linking agent compound obtained in this way can be preferably used as a thermally decomposable internal cross-linking agent in the manufacturing process of the super absorbent polymer.

A kind of system of acetylene and formaldehyde deep reaction

本发明涉及一种乙炔与甲醛深度反应的系统，包括依次连接的第一炔醛反应釜、第二炔醛反应釜、第三炔醛反应釜、过滤系统进料泵、过滤系统、回收系统，所述第一炔醛反应釜分别通过进料和出料管线连接甲醛、催化剂、原料乙炔和乙炔尾气总管，所述第二炔醛反应釜与第三炔醛反应釜均分别通过进料和出料管线连接原料乙炔、过滤系统进料泵、过滤系统、回收系统和乙炔尾气总管。本发明为三级炔醛反应工艺流程，每个釜反应深度不同，反应产物中甲醛浓度逐渐降低，反应温度与压力按梯度进行控制，催化剂在线回收再生与补充，副产聚合物在线排出，适用于连续炔醛化反应：1,4‑丁炔二醇的工业化生产。

Method for preparing acetylenic alcohols using continuous process

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to method for preparing acetylenic alcohols by continuous method. Method involves condensation of ketones of the general formula: R 1 -CH 2 COCH 2 -R 2 with acetylene at temperature about 20-50 C and under pressure about 10-30 kg/cm 2 . Anion-exchange resin is used as a catalyst with groups of quaternary ammonium hydroxide with strong basicity in proton solvent. Feeding reaction mixture is carried out with hour volume rate from 0.1 to 5.0 h -1 . Reaction mixture contains acetylene, ketone and solvent taken in the mole ratio = 1.0 : (0.2- 3.0) : (1.0-4.0), respectively. Ketone comprises substituents R 1 and R 2 that can be similar or different and each means hydrogen atom, linear or branched saturated or unsaturated alkyl comprising 1-16 carbon atoms. Preferably, acetylenic alcohol is prepared taken among the group: 2-methylbut-3-in-2-ol, 3,7-dimethyl-oct-6-ene-1-in-3-ol, 3,7,11-trimethyl-dodeca-6,10-diene-1-in-3-ol, 3,7,11,15- tetramethyl-6,10,14-hexadecatriene-1-in-3-ol and 3,7,11,15-tetramethylhexadeca-1-in-3-ol. As ion-exchange resin Amberlite-402 or Amberlite-900, resin AB-17-8 in OH - -form is used. Aprotonic solvent is taken among the group consisting of dimethylformamide, dimethyl- sulfoxide and N-methylpyrrolidone. Invention provides carrying out the process under mild conditions with high yields of the end product and minimal amount of harmful waste of production. EFFECT: improved preparing method. 11 cl, 14 tbl, 8 dwg, 14 ex _ Сэ сс ПЧ сэ РОССИЙСКОЕ АГЕНТСТВО ПО ПАТЕНТАМ И ТОВАРНЫМ ЗНАКАМ (19) (51) МПК? ВИ "” 2 216 532 ' 13) С2 С 07С 33/042, 29/44 12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ РОССИЙСКОЙ ФЕДЕРАЦИИ (21), (22) Заявка: 99118306/04, 24.08.1999 (24) Дата начала действия патента: 24.08.1999 (30) Приоритет: 26.08.1998 КК 98-34685 (46) Дата публикации: 20.11.2003 (56) Ссылки: КУ 2059597 СЛ, 10.05.1996. КЦ 1240011 СЛ, 27.03.1997. КЦ 1779009 СЛ, 09.02.1995. (98) Адрес для переписки: ...

METHOD OF OBTAINING 2-BUTYL-1-TERM

1344653 Alcohols and esters L GIVAUDAN & CIE SA 10 Nov 1971 [10 Nov 1970] 52176/71 Heading C2C [Also in Division A5] The invention comprises compounds of the formula where R<SP>1</SP> is H or methyl, R<SP>11</SP> is H or alkanoyl of 1-3 carbon atoms, R<SP>111</SP> is butyl, Z is -C#C-, -CH=CH- or -CH 2 -CH 2 - and n is 0-2. The compounds are prepared by .reacting together compounds of the formula and MZR<SP>1</SP> where M is an alkali metal or MgX where X is halogen, provided that M is an alkali metal only when Z is -C#C-, and alkanoylating or hydrogenating the product if desired.

Process for preparing alkyne diols or mixtures of alkyne diols with alkyne monools

Alkindiole oder Gemischen von Alkindiolen mit Alkinmonoolen werden durch Umsetzung von Acetylen mit mehr als äquimolaren Mengen an Ketonen und/oder Aldehyden in Gegenwart einer Alkaliverbindung hergestellt, wobei man die Alkaliverbindung in einer kleineren molaren Menge als der halben molaren Menge des umzusetzenden Ketons und/oder Aldehyds in Gegenwart von Ammoniak und/oder mindestens einem reaktiven primären Amin verwendet.

Subst. cycloptentene perfumery and flavouring materials - prepd. by cyclisation of (2)-oxo-(3,5,9)-decatrienes with conc. sulphuric acid (NL180277)

New substd. cyclopentenes are of formula (I): (where R1 to R6 are H, Me or Et, esp. H or Me). (I) are prepd. by cyclisation of 2-oxo-3,5,9-decatrienes of formula R2-CH2-C(=CHR1)-CHR3-CH2-C(CH2R4)=CH-CH=CR5 -CO-CH2-R6 (II), with concn., esp. 96-98%, H2SO4 at -40 to +20 degrees C. (I) are used as perfumery and flavouring synthetics, to impart hay and green, herbal notes in perfumes, cologne, soaps, foam baths and shampoos. (I) are esp. suitale for shaving lotions and shaving soaps. (I) may also be used for scenting detergents and other consumer articles and for flavouring food, drinks and tobacco. (I) can be prepd. in good yields. In an example a mixt. contg. 40% 4- 2,5,5-trimethyl-cyclopent-2-en-l-ylidene -butan-2-one and 60% 4- 2,5,5-trimethyl-cyclopent-1-en-1-yl -but-3-en-2-one. was prepd. in 58% yield by adding 6,9-dimethyl-3,5,9-decatriene-2-one to 96% H2SO4 and 100 ml hexane at -10 degrees C.

Alkylnols prodn - by reacting acetylenic cpds with carbonyl cpds

Alkynols are prepd. by reacting an acetylenic compd. of formula (II) RC triple bond CH (II) (where R = H, alkyl, aryl or carbinol) with a carbonyl compd. of formula (III) (R1 = alkyl or alkenyl; R2 = H, alkyl or alkenyl), a cycloalkanone or phenylalkanone in liq. NH3, in the presence of an anion exchange resin based on quat. ammonium hydroxide. (I) are inters. for isoprenes, medicaments such as vitamin A and vitamin E, certain terpenes useful in perfumery such as linalol and geraniol, materials for the prodn. of synthetic musks, reticulation agents and catalysts.

15-Trifluoromethyl-15-hydroxy prostanoic acids - with prostaglandin-like activity

Cpds of formula (I): (where one of R1 and R2 is H and the other is free or functionally modified OH, or R1+R2 is free or functionally modified oxo; R3 is free or functionally modified OH; one of R4 and R5 is CF3 and the other is free or functionally modified OH; R6 is 5-10C alkyl or alkenyl; R7 are H or together form a bond; A is vinylene) and their optical isomers, salts and esthers are new. They can be prepd. e.g. by reacting a cpd (II): with X1(CH2)4COOH (where X1 is a phosphonium gp).

Patent FR2338238B1

Process for the preparation of unsaturated carbonyl compounds

Patent FR2361322B1

NEW AROMATIC COMPOSITIONS CONTAINING CARBOXYLIC ACID DERIVATIVES

NOVEL 15-DEOXY-16-HYDROXY-PROSTAGLANDINS, THEIR PRODUCTION PROCESS AND MEDICAMENTS CONTAINING THEM

L'invention a trait au domaine de la chimie pharmaceutique. Elle concerne de nouvelles 15-déoxy-16-hydroxy-prostaglandines et leur procédé de production. Les composés de l'invention sont des analogues des prostaglandines naturelles. Ils peuvent donc être utilisés sous la forme de médicaments. The invention relates to the field of pharmaceutical chemistry. It relates to novel 15-deoxy-16-hydroxy-prostaglandins and their production process. The compounds of the invention are analogs of natural prostaglandins. They can therefore be used in the form of drugs.

PROPARGYL ALCOHOL, CORRESPONDING ALLYL ALCOHOL AND CORRESPONDING KETONE D, E-UNSATURAE AND THEIR PREPARATION PROCESS

NEW ALIPHATIC CARBONYL COMPOUNDS AND THEIR PREPARATION

La présente invention concerne de nouveaux composés carbonyle aliphatiques et leur préparation. Les composes de l'invention répondent à la formule générale : The present invention relates to novel aliphatic carbonyl compounds and their preparation. The compounds of the invention correspond to the general formula:

PROCESS FOR PREPARING UNSATURATED KETONES

Patent FR1573026A

Patent FR2113740A5

Process for the preparation of hexaenes

Process for the synthesis of alkynols

Improvements relating to defoliants

Patent FR2473509B1

Process for the preparation of new acetylene carbinols

ALKYNE-DIOLS-10,15, THEIR PREPARATION PROCESS AND THEIR APPLICATION TO THE PREPARATION OF SQUALANE

Patent FR2430403B1

Manufacturing process of phenyl-alkyne-diols

Patent FR2236822B1

Process for the preparation of a continuous phase silica gel catalyst for the manufacture of alkynols

PROCESS FOR PREPARING STEREOSPECIFIC ISOMERS OF FARNESYLACETIC ACID, ITS ESTERS AND THEIR DERIVATIVES

ALLYL ALCOHOL AND ITS PREPARATION PROCESS

On fournit des alcools allyliques substitués de formule générale (II) : Substituted allyl alcohols of general formula (II) are provided:

NEW 15-DESOXY-16-VINYL- AND 16-CYCLOPROPYLPROSTAGLANDINS E ALKYL ESTERS, USEFUL IN PARTICULAR AS HYPOTENSORS, AND THEIR PREPARATION PROCESS

LES MEDICAMENTS SELON L'INVENTION SONT DES PROSTAGLANDINES E OPTIQUEMENT ACTIVES DE FORMULE GENERALE: (CF DESSIN DANS BOPI) (CF DESSIN DANS BOPI) OU SON IMAGE SPECULAIRE ET LES MELANGES RACEMIQUES, DANS LAQUELLE R EST UN GROUPE METHYLE OU ETHYLE, R EST UN GROUPE ALKYLE EN C-C, T EST UN RADICAL DIVALENT DE FORMULE: (CF DESSIN DANS BOPI) (CF DESSIN DANS BOPI) DANS LAQUELLE R EST UN GROUPE VINYLE OU CYCLOPROPYLE, Z EST UN GROUPE -CH- OU CIS-CH-CHCH-(CH)-, C-C REPRESENTE UN GROUPE ETHYLENE OU TRANSVINYLENE. APPLICATIONS: AGENTS HYPOTENSEURS, BRONCHODILATATEURS, ANTI-INFLAMMATOIRES ET DIVERSES APPLICATIONS DES PROSTAGLANDINES.

Ethynyl carbinol prepn. from unsatd. ketones - pref. methyl vinyl ketone, by ethynylation with magnesium acetylene complex in liq. ammonia

Preparation of ethynyl carbinols

Process for recovering hydrogen in tail gas in production of 1, 4-butanediol

本发明公开了一种1，4‑丁二醇生产时尾气中氢的回收工艺，包括以下步骤：1）粗BDO的制备：通过电石以及甲醇作为原料合成BYD，然后BYD通过还原反应得到粗BDO以及第一驰放气；2）BDO的精制：所述粗BDO经过闪蒸分离得到精制的BDO，同时释放出第二驰放气；3）驰放气的回收：31）第一驰放气的处理：第一驰放气经减压、冷却分离后得到第一氢气；32）第二驰放气的回收：第二驰放气经冷却分离后加压得到第二氢气；33）氢气的回收：分别将第一氢气、第二氢气输送至合成氨系统的变换工段，作为合成氨制备的原料。本发明能够回收利用一种1，4‑丁二醇生产中的氢气，用于合成氨的生产，实现了资源的循环利用。

Preparation of acetylenic alcohols

AN ACETYLENIC ALCOHOL IS PREPARED BY REACTING A KETONE WITH LIQUIFIED ACETYLENE IN THE PRESENCE OF A CO-CATALYST SYSTEM COMPRISING LIQUID AMMONIA AND AN ALKALI METAL HYDROXIDE.

Prepn. of individual farnesylacetic acid (esters) geometric isomers - by rectification of isomer mixts. obtd. from nerolidol

Process for prepg. specific stereoisomers of farnesylacetic aced or its esters of formula (I): CH3. C(CH3)=CH.CH2CH2. C(CH3)DELTA8=CH. CH2CH2. C(CH3)DELTA4= CHCH2CH2COOR2 (I) (R2 = H, 1-6C alkyl, 3-6C cycloalkyl, 2-6C alkenyl or 3-6C cycloalkenyl)comprises rectifying a mixt. of (i) DELTA4,8-cis and DELTA4-trans-DELTA-cis (I); (ii) DELTA4,8-trans (I) or (III) all 4 isomers to recovery from mixts. (i) and (ii) both components and from (iii) the DELTA4,8-cis isomers. Similar processes for separg. DELTA6-cis and DELTA6-trans isomers of nerolidol (II) and DELTA5-cis and DELTA5-trans geranylacetone (III) are also new. (I) are anti-ulcer agents (for which purpose individual isomers are pref), perfumes and aroma agents. (II) and (III) are intermediates for (I), perfumes and cpds. with juvenile hormone activity; (II) is also used to make isophytol a starting material for Vitamin E. Recovery of individual isomers is almost quantitative.

Process for the production of acetylene monoalcohols

PROCESS FOR THE PREPARATION OF ALKYNICALLY UNSATURATED ALCOHOLS.

1-Hydroxymethyl-1-oxo-prostane derivatives of the E, A and F series

The invention disclosed relates to pharmacologically active prostaglandin derivates of the E, F, or A series having on the terminal methylene carbon of the alpha chain a substituent selected from the group consisting of: wherein R is an alkyl group and R 13 is C 1 -C 4 alkyl, di-C,-C. -alkylamino, C 1 -C 4 alkoxy, and phenyl or phenyl substituted with one or more substituents from the group consisting of C 1 -C 4 , OR, SR, F, or Cl wherein R is as previously defined.

Alkynes.

METHOD OF PERFORMING AN EXOTHERMAL REACTION BETWEEN A GAS AND A LIQUID.

Process for the production of methylbutinol

本发明的主题是用于生产甲基丁炔醇的方法，其中该方法包括至少一个渗透蒸发的步骤。在优选的实施方式中，该方法包括以下步骤：(a)提供包含甲基丁炔醇和水的进料组合物，(b)使所述进料组合物在蒸馏装置中进行蒸馏，(c)从所述蒸馏装置除去侧流，所述侧流比所述进料组合物具有较高的水含量，以及(d)使所述侧流进行渗透蒸发，从而减少所述水含量。本发明还涉及用于从甲基丁炔醇除去水或者用于纯化甲基丁炔醇的渗透蒸发和/或渗透蒸发膜的应用。

It is spray-dried butynediols catalyst

一种形成乙炔化催化剂的工艺，包括提供一种水基悬浮液，一种含铜物质，一种含铋物质，一种结构化物质，一种粘结剂。将悬浮液进行喷雾干燥形成颗粒，然后焙烧颗粒形成乙炔化催化剂。

Atom-economic waste-free method of producing 2-(4-fluorphenyl)-but-3-in-2-ola

FIELD: chemistry. SUBSTANCE: method consists in reacting 4-fluoroacetophenone with an acetylenic compound in the presence of solvents. The acetylene compound is gaseous acetylene and, as a solvent, dimethylsulfoxide containing 0.1-0.5% of water, the process is carried out in the presence of a catalytic system, which is prepared by preheating hydrated potassium hydroxide, diethylene glycol and dimethylsulfoxide at a molar ratio of 4-fluoroacetophenone: KOH×0.5H 2 O: diethylene glycol of 1:0.25-1.0:0.5-1.0, at the temperature of 100-120°C for 0.5-1.0 h, the main reaction is carried out at the temperature of 10-20°C for 1-4 hours, and the desired product is isolated by extraction with diethyl ether, followed by distillation in vacuum. EFFECT: obtaining the target alcohol with a yield of 91 percent. 8 ex РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2 629 024 C1 (51) МПК C07C 29/42 (2006.01) C07C 33/48 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ (21)(22) Заявка: 2016117649, 04.05.2016 (24) Дата начала отсчета срока действия патента: 04.05.2016 Дата регистрации: Приоритет(ы): (22) Дата подачи заявки: 04.05.2016 (45) Опубликовано: 24.08.2017 Бюл. № 24 вторичных пропаргиловых спиртов из ароматических и гетероароматических альдегидов и ацетилена в системе КОН-Н 2 О-ДМСО. ЖОргХ, 2013, т.49, вып.3, стр. 369-372. RU 2479565C1, 20.04.2013. US 6147266A1, 14.11.2000. JP 51075013A, 29.06.1976. R U (54) Атом-экономный безотходный способ получения 2-(4-фторфенил)-бут-3-ин-2-ола (57) Реферат: Изобретение относится к способу получения процесс проводят в присутствии каталитической 2-(4-фторфенил)-бут-3-ин-2-ола, который может системы, которую получают предварительным быть использован для получения изопреноидов, нагреванием гидратированного гидроксида калия, каротиноидов, витаминов А и E, ароматических диэтиленгликоля и диметилсульфоксида при композиций, противоклещевых агентов, мольном соотношении 4-фторацетофенон: гербицидов, ингибиторов ...

Propargyl sulfone compound and preparation method and application thereof

本发明公开了一种炔丙基砜类化合物及其制备方法与应用。本发明通过将炔醇加入反应溶剂中，按反应摩尔比再加入亚磺酸底物，在温和的反应温度下搅拌进行反应，将得到的反应体系除去反应溶剂后进一步纯化后得到炔丙基砜类化合物。本发明制备方法所需反应条件十分温和、绿色，原子经济性高，适用的底物范围广泛，所得到的炔丙基砜类化合物有潜在的药物活性和生物活性，是在生物和药物活性分子中广泛存在的重要骨架，例如存在于组织蛋白抑制剂、癌症抑制剂，DNA切断剂、除草剂等生物和药物活性分子中。

Method for addition reaction of acetylene and ketone compound

The disclosure discloses a method for an addition reaction of acetylene and a ketone compound. The method includes the following steps: S1, providing a continuous reaction device, wherein the continuous reaction device includes a plurality of bubble tubular reactors being connected with each other through connecting tubes; feeding a raw material solution containing the ketone compound and alkali into the plurality of bubble tubular reactors, and S3, under normal pressure, pumping acetylene from the bottom of the first bubble tubular reactor for the addition reaction. By applying the technical solution of the invention, acetylene reacts with the ketone compound in the plurality of bubble tubular reactors arranged in series, which can ensure the sufficient gas-liquid contact time, and thus making full use of the acetylene gas, improving the utilization rate thereof, effectively reduing the amount of acetylene, reducing costs, and further improving the safety.

Treprostinil production

The present invention is directed to a novel method for preparing a synthetic intermediates for treprostinil. Also described are methods of preparing treprostinil comprising utilizing novel intermediates described herein as well as novel intermediates useful for synthesis prostacyclin derivatives, such as treprostinil.

Novel 11-hydroxy-9-keto-5,6-cis-13,14-cis-prostadienoic acid derivatives

This disclosure describes certain 11-hydroxy and 11-deoxy-9-keto(or hydroxy)-prostanoic acid derivatives useful as bronchodilators, hypotensive agents, anti-ulcer agents, or as intermediates.

NOVEL 15-DEOXY-16-HYDROXY-PROSTAGLANDINS ESTERIFIED IN POSITION 1, PROCESS FOR THEIR PRODUCTION AND MEDICAMENT CONTAINING SAME

L'invention a trait au domaine de la chimie pharmaceutique. Elle concerne de nouvelles 15-déoxy-16-hydroxy-prostaglandines estérifiées en position 1 et leur procédé de production par réaction d'un organolithiocuprate sur une 2-cyclopentène-1-one substituée en positions 2 et 4. Les composés de l'invention sont des analogues des prostaglandines naturelles. Ils peuvent donc être utilisés sous la forme de médicaments. The invention relates to the field of pharmaceutical chemistry. It relates to novel 15-deoxy-16-hydroxy-prostaglandins esterified in position 1 and their production process by reaction of an organolithiocuprate with a 2-cyclopentene-1-one substituted in positions 2 and 4. The compounds of the invention are analogues of natural prostaglandins. They can therefore be used in the form of drugs.

Patent FR2292464B1

A kind of chain yne compounds and its synthetic method

本发明涉及链状烯炔类化合物，所述化合物化学结构式为： 其中，取代基R 1 和R 2 为苯基或对甲基苯基或氢或对甲基或乙基或异丙基或对甲氧基苯基或异己基，取代基R 3 为氢或2,4‑二氯苯基或甲基或环丙基或异丙基或正丁基，取代基位置、个数以及共轭位置不固定。合成方法为以一类简单易得的炔醇为原料，在路易氏酸的催化下合成各种重要的链状烯炔类化合物。该发明关键点在于提供了一种步骤少、产率高的合成新方法以合成一类新型链状烯炔类化合物，又因产物分子结构中同时存在烯键和炔键两个活性官能团，兼有这两类化合物的基本性质，在有机合成中可以发生重要的加成反应、环化反应、偶联反应等重要的反应合成各种目标化合物。

Cis-prostaglandin-like compounds and methods of making

A kind of preparation of copper bismuth/SiO 2 catalyst

发明涉及一种铜铋/二氧化硅催化剂的制备。其特征在于以“一锅法”制备了铜铋/二氧化硅催化剂，氧化铜含量为10‑40%,铋含量为1‑10%，其余为二氧化硅。铜铋物种高分散在二氧化硅内外表面，提高了催化剂的反应中心，增强了催化剂的耐磨性，减少了铜离子的脱溶度。在炔醛化反应合成1,4‑丁炔二醇的应用中，铜铋催化剂活性好，选择性高，铜物种脱溶量较低。

Patent FR2109559A5

Process for the separation and production of propargyl alcohol

Verfahren zur Abtrennung und Gewinnung von Propargylalkohol, dadurch gekennzeichnet, dass ein Propargylalkohol enthaltendes Produktgemisch, das durch Umsetzung von Paraformaldehyd mit Acetylen in Gegenwart eines Katalysators in einem polaren Lösungsmittel erhalten wurde, einer Destillation bei einem Druck von 100 bis 150 mm Hg unterzogen wird. Process for the separation and recovery of propargyl alcohol, characterized in that a product mixture containing propargyl alcohol, which was obtained by reacting paraformaldehyde with acetylene in the presence of a catalyst in a polar solvent, is subjected to distillation at a pressure of 100 to 150 mm Hg.

Intermediates for prostaglandin synthesis

Abstract of the Disclosure Compounds of the formula

Furanone meat flavor compositions

(6R,10R)-6,10,14-trimetylpentadecan-2-one prepared FROM (R)-6,10,14-trimetylpentadec-5-en-2-one

本发明涉及一种以多步合成的方式由(R)-6，10-14-三甲基十五碳-5-烯-2-酮的E/Z异构体的混合物制备(6R，10R)-6，10，14-三甲基十五烷-2-酮的方法。所述方法是非常有利的，因为其以有效的方式由起始产物的立体异构体混合物形成期望的手性产物。

Process for the preparation of 6-methyl-3-hepten-2-one, and process for the preparation of phyton or isophytol

DIAZOLYLALKANOLER, FOERFARANDE FOER DERAS FRAMSTAELLNING OCH DERAS ANVAENDNING SAOSOM ANTIMYKOTISKA MEDEL

Method for synthesizing propiolic alcohol

一种合成丙炔醇的方法，采用多聚甲醛为甲醛原料来源，以氢氧化钾或醇钾为催化剂，在芳香烃或脂肪烃有机溶剂中，与低于0.15MPa压力的乙炔进行反应生成丙炔醇。反应终点物料是“液‑液”两相体系，经沉降分离、水解分离、萃取提纯和精馏分离收取产物，产物中丙炔醇收率可达71%～73%。

Process for the preparation of 3-azolylpropynes and compounds thereby produced

Process for the preparation of alkine diols by the reaction of ketones with acetylene

Alkynediols are obtained by reaction of ketones with acetylene in the presence of a base, which was previously done in organic solvents such as acetaldehyde dibutyl acetal, methylal, dioxane, diisopropyl ether, tetrahydrofuran or hydrocarbons. In most cases, these suspensions are highly viscous. Moreover, conversion of the ketone is in general incomplete. <??>The use of alkyl tert-butyl ethers, preferably methyl tert-butyl ether, as the solvent eliminates the disadvantages and gives high yields in combination with high conversions. <??>Preparation of 2,4,7,9-tetramethyldec-5-yne-4,7-diol, 2,5,8,11-tetramethyldodec-6-yne-5,8-diol.

1-oxo-1-phenyl-hexa-2, 4-diyne and its intermediate and process for the production of said compounds

Method for synthesizing 1, 4-butynediol and coproducing propiolic alcohol by formaldehyde ethynylation

本发明公开一种甲醛乙炔化合成1,4‑丁炔二醇联产丙炔醇的方法，以铜铋复合氧化物为催化剂，反应温度为80~150℃，优选为90~120℃，反应压力为0.2~2.0MPa，优选0.5~1.0 MPa，乙炔的流量为40~200ml/min，优选为80~150 ml/min，甲醛水溶液质量浓度为4%~25%，优选为9%~15%，催化剂用量同加入的甲醛水溶液质量体积比为1:3~1:10，优选为1:5~1:7，所述甲醛水溶液中含有聚乙二醇200，聚乙二醇800，聚乙二醇600，乙二醇，二甘醇，中的一种或几种，优选为乙二醇和二甘醇，其加量为甲醛水溶液重量的0.5%~3.5%，优选0.8~2.0%。该方法能够明显提高丙炔醇的产量，并且运转周期长。

FOER FARING FRAMSTAELLNING AV ALFA-ETYNYL-BENSHYDROLER

Patent JPS492092B1

An efficient process to induce enantioselectivity in procarbonyl compounds

An efficient method to induce the enantioselectivity in procarbonyl compounds using chiral organometallic complexes. The present invention is also described a method for producing organo metallic complexes using a base and a metal halide.

Method for producing 3,7-dimethyl-1-octen-3-ol

本発明は、以下の工程、すなわち、ａ）水素と、炭素、炭酸カルシウムおよび酸化アルミニウムからなる群から選択される担体に担持されたパラジウム含有触媒との存在下において、６−メチル−５−ヘプテン−２−オンを水素化して６−メチル−２−ヘプタノンとする工程と、ｂ）アンモニアと水酸化カリウムとの存在下およびさらなる有機溶媒の不在下において、６−メチル−２−ヘプタノンとアセチレンとを反応させて３，７−ジメチル−１−オクチン−３−オールとする工程と、ｃ）水素と、炭酸カルシウム、酸化アルミニウム、シリカ、多孔質ガラス、炭素またはグラファイト、および硫酸バリウムからなる群から選択される担体に担持されたパラジウム含有触媒との存在下において、３，７−ジメチル−１−オクチン−３−オールを水素化して３，７−ジメチル−１−オクテン−３−オールとする工程であって、但し、この触媒は、担体が炭酸カルシウムである場合は鉛をさらに含有することを条件とする、工程とを包含する、３，７−ジメチル−１−オクテン−３−オールの製造方法に関する。本発明は、さらに、そうして製造された３，７−ジメチル−１−オクテン−３−オールが出発原料として使用される、イソフィトールおよびビタミンＥの製造方法に関する。