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Preparation method of bis(ditert-butyl phenyl phosphine)palladium dichloride

A technology of di-tert-butyl phenyl phosphine and di-tert-butyl phosphorus chloride is applied in the field of precious metal catalyst preparation, and can solve the problems of low process yield, inability to utilize metals and the like, and achieve the effect of high yield

Active Publication Date: 2020-02-07
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing process is mainly based on the direct coordination reaction of the ligand and the metal source. This process has a low yield and cannot effectively utilize the metal.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Prepare phenyl Grignard reagent, the method is as follows: under stirring state, mix magnesium chips, dibromoethane, and anhydrous tetrahydrofuran, seal, heat up to 60°C and reflux, and then add dropwise 50 v / v% of bromobenzene Tetrahydrofuran solution, after the dropwise addition, react at 60°C for 4h, and cool to room temperature naturally; wherein, the molar ratio of magnesium chips, dibromoethane, and bromobenzene is 1:0.1:1.1, and the magnesium The mass ratio of crumbs and anhydrous tetrahydrofuran is 1:5.

Embodiment 2

[0023] A preparation method of two (di-tert-butylphenylphosphine) palladium dichloride, comprising the following steps:

[0024] (1) Dissolve 10g of palladium sponge with aqua regia, filter after concentrating and catching nitrate, and dilute the filtrate with water to obtain a chloropalladium acid solution with a mass concentration of palladium of 15%; then add the chloropalladium acid solution dropwise to 30g 1,5-cyclooctadiene and 150g ethanol in 1,5-cyclooctadiene-ethanol solution, react at 30°C until the precipitate no longer precipitates, cool and filter to obtain 26.75g 1,5-cyclooctadiene Alkene palladium chloride, yield 99.7%; wherein, the mass ratio of palladium in the chloropalladium acid solution to 1,5-cyclooctadiene is 1:3;

[0025] (2) According to the equal molar weight of phenyl Grignard reagent and di-tert-butyl phosphorus chloride, the phenyl Grignard reagent prepared in Example 1 was added dropwise to the tetrahydrofuran solution of di-tert-butyl phosphorus ...

Embodiment 3

[0031] A preparation method of two (di-tert-butylphenylphosphine) palladium dichloride, comprising the following steps:

[0032] (1) Dissolve 10g palladium sponge with aqua regia, filter after concentrating and catching up with nitrate, dilute the filtrate with water to obtain a chloropalladium acid solution with a mass concentration of palladium of 20%; then add the chloropalladium acid solution dropwise to 40g 1,5-cyclooctadiene, 300g ethanol in 1,5-cyclooctadiene ethanol solution, react at 40°C until the precipitate no longer precipitates, cool and filter to obtain 26.77g 1,5-cyclooctadiene Alkene palladium chloride, yield 99.8%; wherein, the mass ratio of palladium in the chloropalladium acid solution to 1,5-cyclooctadiene is 1:4;

[0033] (2) According to the equal molar weight of phenyl Grignard reagent and di-tert-butyl phosphorus chloride, the phenyl Grignard reagent prepared in Example 1 was added dropwise to the tetrahydrofuran solution of di-tert-butyl phosphorus ch...

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PUM

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Abstract

The invention discloses a preparation method of bis(ditert-butyl phenyl phosphine)palladium dichloride. The preparation method includes the following steps that (1) palladium sponge is dissolved in royal water, concentrated, saltpetre-removed and then filtered, and a filtrate is diluted with water to obtain a solution of palladium chloride acid; and then the filtrate is dropwise added into an ethanol solution of 1,5-cyclooctadiene, reacted until precipitation is no longer precipitated, and filtration is conducted to obtain 1,5-cyclooctadiene palladium chloride; (2) a phenyl grignard reagent isdropwise added into a tetrahydrofuran solution of bi tertiary butyl phosphorus dichloride to obtain a tetrahydrofuran solution of bis(ditert-butyl phenyl phosphine); (3) the tetrahydrofuran solutionof the bis(ditert-butyl phenyl phosphine) is dropwise added into a tetrahydrofuran solution of the1,5-cyclooctadiene palladium chloride; (4) filtration is conducted, and a filter cake is washed with anhydrous ethanol; and (5) drying is conducted. According to the preparation method, the 1,5-cyclooctadiene palladium chloride prepared by taking the palladium chloride acid as a metal source is used as a reaction precursor, the prepared bis(ditert-butyl phenyl phosphine) is used as an ligand, the ligand does not require purification, and the yield of products is high.

Description

technical field [0001] The invention belongs to the technical field of preparation of noble metal catalysts, and in particular relates to a preparation method of bis(di-tert-butylphenylphosphine)palladium dichloride. Background technique [0002] Bis(di-tert-butylphenylphosphine)palladium dichloride is an important metal palladium catalyst, widely used in catalyzing C-C bond coupling reactions of Sonogashira, Suzuki, Stille, Heck, etc. exhibits unique advantages. It has a wide range of uses in the synthesis of polymers, liquid crystal materials, functional materials, drugs and compounds with biological activity. [0003] The existing technology is mainly based on the direct coordination reaction of the ligand and the metal source, which has a low yield and cannot effectively utilize the metal. Contents of the invention [0004] The invention provides a method for preparing bis(di-tert-butylphenylphosphine)palladium dichloride, which uses palladium sponge as a metal sourc...

Claims

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Application Information

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IPC IPC(8): C07F15/00
CPCC07F15/0066
Inventor 校大伟曾永康姚琪张宇
Owner XIAN CATALYST NEW MATERIALS CO LTD
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