Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing bis(diphenylphosphino)alkane palladium dichloride complex

A technology of alkane palladium dichloride and diphenylphosphine is applied in the field of preparation of bis(diphenylphosphine) alkane palladium dichloride complex, and can solve the problems of unfriendly environment, high production cost, long reaction process and the like , to achieve the effect of short cycle, low cost and simple synthesis process

Active Publication Date: 2013-08-28
XIAN CATALYST NEW MATERIALS CO LTD
View PDF6 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current synthesis method of bis(diphenylphosphine)alkane palladium dichloride is mainly obtained by ligand exchange with bis(diphenylphosphine)alkane through acetonitrile palladium chloride complex intermediate, which involves Acetonitrile is a highly toxic substance, and the reaction process is lengthy, the production cost is high, and the environment is not friendly

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Step 1. Add aqua regia (concentrated hydrochloric acid and concentrated nitric acid in a volume ratio of 3:1) to 10.0g sponge palladium. After the sponge palladium is completely dissolved, add 37% by mass to the dissolved solution. Concentrated hydrochloric acid until brown nitrogen oxide compounds no longer emerge in the solution, filter the solution, and concentrate the filtrate obtained by the filtration into a chloropalladic acid solution with a palladium concentration of 0.4g / mL;

[0017] Step 2. Add 45.0g of 1,2-bis(diphenylphosphine)ethane to 300mL of N,N-dimethylformamide and heat to 60℃ to obtain N,N- of bis(diphenylphosphine)alkane Dimethylformamide solution;

[0018] Step 3. Add the chloropalladium acid solution described in step one to the N,N-dimethylformamide solution of bis(diphenylphosphine) alkane described in step two under stirring conditions. After the addition is complete React for 90 min under stirring conditions at a temperature of 60°C, and filter af...

Embodiment 2

[0022] Step 1. Add aqua regia (concentrated hydrochloric acid and concentrated nitric acid in a volume ratio of 3:1) to 10.0g sponge palladium. After the sponge palladium is completely dissolved, add 37% by mass to the dissolved solution. Concentrate hydrochloric acid until the brown nitrogen oxide compounds no longer emerge in the solution, filter the solution, and concentrate the filtrate obtained by the filtration into a chloropalladic acid solution with a palladium concentration of 0.3g / mL;

[0023] Step 2. Add 45.0g of 1,3-bis(diphenylphosphine)propane to 400mL of N,N-dimethylformamide and heat to 50°C to obtain N,N-bis(diphenylphosphine)alkane Methylformamide solution;

[0024] Step 3. Add the chloropalladium acid solution described in step one to the N,N-dimethylformamide solution of bis(diphenylphosphine) alkane described in step two under stirring conditions. After the addition is complete React for 60 minutes under stirring conditions at a temperature of 50°C, and filter...

Embodiment 3

[0028] Step 1. Add aqua regia (concentrated hydrochloric acid and concentrated nitric acid in a volume ratio of 3:1) to 10.0g sponge palladium. After the sponge palladium is completely dissolved, add 37% by mass to the dissolved solution. Concentrated hydrochloric acid until brown nitrogen oxide compounds no longer emerge in the solution, filter the solution, and concentrate the filtered filtrate into a chloropalladic acid solution with a palladium concentration of 0.5 g / mL;

[0029] Step 2: Add 44.0g of 1,4-bis(diphenylphosphine)butane to 400mL of N,N-dimethylformamide and heat to 50°C to obtain the N,N- of bis(diphenylphosphine)alkane Dimethylformamide solution;

[0030] Step 3. Add the chloropalladium acid solution described in step one to the N,N-dimethylformamide solution of bis(diphenylphosphine) alkane described in step two under stirring conditions. After the addition is complete React for 60 minutes under stirring conditions at a temperature of 50°C, and filter after the ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for preparing a bis(diphenylphosphino)alkane palladium dichloride complex. The method comprises the steps of: (1) preparing a chloropalladite solution; (2) adding bis(diphenylphosphino) alkane into N,N-dimethylformamide so as to prepare a N,N-dimethylformamide solution of bis(diphenylphosphino) alkane; (3) dropwise adding the chloropalladite solution to the N,N-dimethylformamide solution of bis(diphenylphosphino) alkane while stirring, carrying out stirring reaction after the dropwise adding process is completed, and filtering after cooling so as to obtain a filter cake; and (4) washing the filter cake, and carrying out vacuum drying on the washed filter cake, thereby obtaining the bis(diphenylphosphino)alkane palladium dichloride complex. According to the method, palladium sponge is directly adopted as a palladium source, the target product is synthesized from chloropalladite and a ligand, namely the bis(diphenylphosphino) alkane, in a DMF (N,N-dimethylformamide) solvent in one step, and a process for preparing intermediates, namely palladium chloride and acetonitrile palladium chloride, is avoided, so that the method has the characteristics of simple synthesis process, short cycle, low cost and the like.

Description

Technical field [0001] The invention belongs to the technical field of organic catalysis and the preparation of precious metal catalysts for medical synthesis, and specifically relates to a preparation method of a bis(diphenylphosphine) alkane palladium dichloride complex. Background technique [0002] Bidentate phosphine ligand metal complexes have received extensive attention from researchers because of their special structure and novel catalytic performance. Bis(diphenylphosphine)alkane palladium dichloride, including 1,2-bis(diphenylphosphine)ethane palladium dichloride, 1,3-bis(diphenylphosphine)propane palladium dichloride, 1 ,4-bis(diphenylphosphine)butane palladium dichloride, etc., are widely used to catalyze olefin hydrogenation, olefin carbon monoxide carbonylation, coupling and other reactions. [0003] The current synthesis method of bis(diphenylphosphine)alkane palladium dichloride is mainly obtained by ligand exchange between acetonitrile palladium chloride complex ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07F19/00
Inventor 王昭文王盼潘丽娟朱柏烨曾永康张之翔
Owner XIAN CATALYST NEW MATERIALS CO LTD