Benzoyl calixarene bonded silica gel stationary phase, preparation method and application thereof

The invention discloses a benzoyl calixarene bonded silica gel stationary phase which is prepared by the following steps of: taking gamma-(2,3-epoxypropoxy) propyl trimethylsilicane as a coupling agent, under the protection of the catalyst and inert gas, reacting with the silica gel so as to prepare gamma-glycidol ether bonded silica gel; then under strong alkaline conditions and the protection of the catalyst and the inert gas, reacting with benzoyl calicanee sodium phenolate so as to prepare the benzoyl calixarene bonded silica gel stationary phase; and finally sealing tail by trimethylsilicane. As the prepared benzoyl calixarene bonded silica gel stationary phase is high in bonded amount, stable in performance, and better in separation selectivity; the benzoyl calixarene bonded silica gel stationary phase has traditional ODS (Octadecylsilyl) reversion phase chromatography performance, and can provide many action sites containing complexing action, hydrogen bonding action and the like ...

Application of cyclopalladated ferrocenylimine-phosphine adduct in synthesis of asymmetric biaryl compound

The invention belongs to the technical field of organic synthesis, and in particular relates to an application of a cyclopalladated ferrocenylimine-phosphine adduct in synthesis of an asymmetric biaryl compound. In synthesis of the asymmetric biaryl compound, the cyclopalladated ferrocenylimine-phosphine adduct is utilized as a catalyst, and the catalyst has the advantages of good stability, efficient catalytic activity and wide applicability; and by utilizing the catalyst, a corresponding coupling product with high yield (up to 95%) can be obtained on the premise of smaller catalytic amount, and the synthesis process has the characteristics of mild reaction conditions, wide substrate range and strong reaction specificity.

Chiral and non-chiral diimidazolinylbenzene compounds and synthesis method

Method for synthesizing aryl radical nitrile derivant under catalysis of cyclopalladated ferrocenylimines complex

The invention pertains to the synthesizing technology field of organic intermediate, relating to a synthesizing method of derivative of aryl nitrie by the catalysis of cyclopalladated ferrocenylimine complex; the preparation steps are that: catalyst, potassium ferrocyanide and alkali are dissolved into an organic solvent, then halonitroaromatic compound is added to be reacted in the protection of nitrogen, and is cooled down to room temperature after the reaction is completed, the product can be acquired after the mixture being washed with water, extracted, dried, concentrated and purified. The reaction uses the universal catalyst, wherein Y is H or CH3; Z is H, CH3, OCH3 or OC2H5. The invention has the advantages of mild reaction conditions, universal material scope, good reaction specificity, high yielding and free of environmental pollution.

A Cyclo palladium diferrocenyl imine amino phosphine compound and an application thereof

Ferrocenyl cycloimine palladium-phosphine adduct and preparation and application therefore

The invention belongs to synthesis of a catalyst and application therefore in organic synthesis, in particular to a ferrocenyl cycloimine palladium-phosphine adduct and preparation and application thereof. In the synthesis of arylboronic acid ester, the ferrocenyl cycloimine palladium-phosphine adduct is used as a catalyst which has favorable stability, high-efficiency catalytic activity and wide applicability and can be used for synthesizing a corresponding coupling product with high yield (as high as 93 percent) on the premise of lower catalytic amount. The invention has the advantages of mild reaction condition, wide substrate range and strong reaction specificity.

Ferrocenyl imidazoliny palladium compound, its preparation method and its uses in catalytic synthesis of coupling product

Method for selectively synthesizing single chiral or double chiral ferrocenyl amine

The invention belongs to the field of chiral compound synthesis, in particular to a novel method for selectively synthesizing single or double chiral ferrocenylamines. The method comprises: adding sodium borohydride into an alcobolic solution of a ferrocenylimine compound at a temperature of no more than 5 DEG C, stirring the mixture for reaction for 7 to 10 hours, and obtaining a ferrocenyl sec-amine compound by separating and purifying products obtained after the reaction; and preparing an alcobolic solution of the ferrocenyl sec-amine, adding ammonium formate and a palladium-carbon catalyst into the alcobolic solution, heating the solution for refluxing for 1 to 3 hours, and obtaining the single or double chiral ferrocenylamines after post treatment. The method uses cheap sodium borohydride as a reducing agent, simplifies reaction steps, reduces reaction cost, requires mild reaction conditions, is easy to synthesize industrially and achieves 99 percent of diastereomers.

Tetraazacalix arene triazine bonded silica gel stationary phase and preparation method and application thereof

The invention discloses a tetraazacalix [2] arene [2] triazine bonded silica gel stationary phase with high bonding quantity and stable bonding layers. A preparation method for the stationary phase comprises that: 3-aminopropyltriethoxysilane silica gel and tetraazacalix [2] arene [2] triazine undergo reflux reaction in N2 at the temperature of 130 DEG C in the presence of anhydrous potassium carbonate to form the tetraazacalix [2] arene [2] triazine bonded silica gel stationary phase. The calixarene bonded stationary phase synthesized by adopting the method has high bonding quantity and stable bonding layers; and the preparation method is simple and convenient, has low preparation cost and wide application range. The stationary phase not only has the reversed phase chromatography performance of the traditional ozone depleting substance (ODS), but also can provide multiple acting sites of complexing, hydrogen bonding effect, phi-phi effect, spatial matching and the like, so the stationary ...

Ferrocenyl cycloimine palladium-phosphine adduct and preparation and application therefore

The invention belongs to synthesis of a catalyst and application therefore in organic synthesis, in particular to a ferrocenyl cycloimine palladium-phosphine adduct and preparation and application thereof. In the synthesis of arylboronic acid ester, the ferrocenyl cycloimine palladium-phosphine adduct is used as a catalyst which has favorable stability, high-efficiency catalytic activity and wideapplicability and can be used for synthesizing a corresponding coupling product with high yield (as high as 93 percent) on the premise of lower catalytic amount. The invention has the advantages of mild reaction condition, wide substrate range and strong reaction specificity.

Method for synthesizing aryl radical nitrile derivant under catalysis of cyclopalladated ferrocenylimines complex

The invention pertains to the synthesizing technology field of organic intermediate, relating to a synthesizing method of derivative of aryl nitrie by the catalysis of cyclopalladated ferrocenyliminecomplex; the preparation steps are that: catalyst, potassium ferrocyanide and alkali are dissolved into an organic solvent, then halonitroaromatic compound is added to be reacted in the protection ofnitrogen, and is cooled down to room temperature after the reaction is completed, the product can be acquired after the mixture being washed with water, extracted, dried, concentrated and purified. The reaction uses the universal catalyst, wherein Y is H or CH3; Z is H, CH3, OCH3 or OC2H5. The invention has the advantages of mild reaction conditions, universal material scope, good reaction specificity, high yielding and free of environmental pollution.

heterocyclic polymer-contg. carried palladium complex and use thereof in Heck reaction

A heterocycle-containing high-molecular material carried metal Pd complex is prepared from polyacrylic nitrile as skeleton, grafting or cross-linking by imidazoline or oxazoline, and reacting with metal Pd salt. It can be used in Heck reaction with high catalyst efficiency, simple operation, cyclic use and no pollution.

Heterocyclic polymer-contg. carried palladium complex and use thereof in Heck reaction

Calixarene crown ether bonded silica stationary phase and preparation method and application thereof

The invention discloses a calixarene crown ether bonded silica stationary phase. Gamma-(2,3-epoxypropoxy)propyltrimethoxy silane is used as a coupling agent which reacts with silica under the protection of catalyst and inert gas to prepare gamma-glycidoxy propyl-bonded silica; and the gamma-glycidoxy propyl-bonded silica reacts with p-tert-butylcalix[4]-1,2-crown-4 sodium phenolate in strong alkaline conditions and under the protection of catalyst and inert gas to obtain the calixarene crown ether bonded silica gel stationary phase. Due to large bonding quantity, stable performance and better separation selectivity, the stationary phase disclosed by the invention not only has the traditional ODS (octadecylsilane bonded silica) reversed-phase chromatography performance, but also can provide sites for various actions such as complexing action, hydrogen bonding and the like; and the stationary phase has remarkable advantages in separating some specific substances which are difficult to separate ...

Method for synthesizing triarylmethane and derivatives

PROCESS FOR PREPARING BENZO-CROWN ETHERS

... 本发明是对佩德森苯并冠醚合成方法的改进，其特征是睚密闭体系中加热反应物，以适当提高反应压力，使之在使用一般溶剂的情况下，实现反应温度的提高，从而加速反应，使常用苯并冠醚的合成反应时间显著缩短，仅为佩德森方法的十分之一到四分之一，达到了与其相当或较高的产率水平，产品质量良好，可实现工业化批量生产。 ...