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Preparation method for bis[di-tert-butyl(4-dimethylaminophenyl)phosphine]dichloropalladium

A technology of dimethylaminophenyl and dimethylaminophenylphosphine, which is applied in the field of phosphine palladium preparation, can solve the problems of high consumption of noble metal palladium, high risk factor of lithium reagent raw materials, high synthesis cost, etc., and achieve high yield effect

Inactive Publication Date: 2018-10-16
陕西瑞科新材料股份有限公司
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  • Abstract
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Problems solved by technology

[0006] The purpose of this invention is to provide a kind of preparation method of dichlorodi-tert-butyl-4-dimethylaminophenylphosphine palladium, solve existing dichlorodi-tert-butyl-(4-dimethylaminophenyl) In the preparation process of phosphine palladium, the consumption of precious metal palladium is large, the risk factor of using lithium reagent raw materials is high, and the synthesis cost is high.

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  • Preparation method for bis[di-tert-butyl(4-dimethylaminophenyl)phosphine]dichloropalladium
  • Preparation method for bis[di-tert-butyl(4-dimethylaminophenyl)phosphine]dichloropalladium
  • Preparation method for bis[di-tert-butyl(4-dimethylaminophenyl)phosphine]dichloropalladium

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preparation example Construction

[0042] Such as figure 1 Shown, is the reaction mechanism figure of a kind of dichlorodi-tert-butyl-4-dimethylaminophenylphosphine palladium preparation method of the present invention, specifically comprises the following steps:

[0043] In step 1, the Grignard reagent is prepared by using N,N-dimethyl-p-haloaniline and magnesium chips with a raw material molar ratio of 1:1-1.5.

[0044] Step 1.1, Initiation of the Grignard Reaction

[0045] Under the protection of nitrogen, add magnesium chips, then add anhydrous tetrahydrofuran that has just been covered with magnesium chips, then drop N,N-dimethyl p-haloaniline in anhydrous tetrahydrofuran solution (add in every liter of anhydrous tetrahydrofuran 160g-210g of N,N-dimethyl-p-chloroaniline), add 0.1-0.5g iodine grains, heat up to 45°C-55°C and stir, the Grignard reaction is triggered, stop heating;

[0046] Step 1.2, continue to drop the anhydrous tetrahydrofuran solution of N,N-dimethyl p-haloaniline in the solution of ste...

Embodiment 1

[0058] Take a dry 10L four-necked reaction flask, fully replace it with dry nitrogen and under the protection of dry nitrogen flow, add 150g of magnesium chips whose surface oxide layer has been removed, then add 200mL of anhydrous tetrahydrofuran to cover the magnesium chips, and then add N, N - 50-80mL of anhydrous tetrahydrofuran solution of dimethyl-p-chloroaniline (800g of N,N-dimethyl-p-chloroaniline is dissolved in 5L of anhydrous tetrahydrofuran); then add 0.5g of iodine, stir and heat up to 50°C , after the Grignard reaction is triggered, stop heating; continue to dropwise add the anhydrous tetrahydrofuran solution of N,N-dimethyl-p-chloroaniline, the dropping speed is to maintain the temperature of the reaction system at 60°C, and keep the temperature at 60°C for 1h after the dropwise addition , take a sample to detect the remaining amount of raw material N,N-dimethyl-p-chloroaniline, if the remaining mass of N,N-dimethyl-p-chloroaniline does not exceed 0.1%, the prep...

Embodiment 2

[0063] Take a dry 10L four-necked reaction flask, fully replace it with dry nitrogen and under the protection of dry nitrogen flow, add 150g of magnesium chips whose surface oxide layer has been removed, then add 200mL of anhydrous tetrahydrofuran to cover the magnesium chips, and then add N, N - 50-80 mL of anhydrous tetrahydrofuran solution of dimethyl-p-bromoaniline (in which 1028.5 g of N, N-dimethyl-p-bromoaniline is dissolved in 5 L of anhydrous tetrahydrofuran); then add 0.3 g of iodine particles, stir and heat up to 45 ℃, after the Grignard reaction is triggered, stop heating; continue to drop the anhydrous THF solution of N,N-dimethyl-p-bromoaniline, the dropping speed is to maintain the temperature of the reaction system at 50°C, and keep the reaction at 50°C after the dropwise addition After 1 hour, take a sample to detect the remaining amount of the raw material N,N-dimethyl-p-bromoaniline. If the remaining mass of N,N-dimethyl-p-bromoaniline does not exceed 0.1%, t...

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Abstract

The invention discloses a preparation method for bis[di-tert-butyl(4-dimethylaminophenyl)phosphine]dichloropalladium. The preparation method comprises the following steps that 1, a Grignard reagent isprepared from the raw materials of N, N-dimethyl p-haloaniline and magnesium chips; 2, the Grignard reagent is taken and cooled, then a catalyst is added for reaction, then di-tert-butylchlorophosphane is dropwise added, and heating is carried out for reaction so as to obtain di-tert-butyl-4-dimethylaminophenylphosphine; 3, the di-tert-butyl-4-dimethylaminophenylphosphine is purified; and 4, complexing bis(acetonitrile)dichloropalladium and the purified di-tert-butyl-4-dimethylaminophenylphosphine so as to obtain a target product. The preparation method has the advantages that the di-tert-butyl-4-dimethylaminophenylphosphine is purified, the high-purity di-tert-butyl-4-dimethylaminophenylphosphine is used for reacting with the bis(acetonitrile)dichloropalladium, and therefore the yield loss of the noble metal palladium is greatly reduced, the preparation cost is greatly lowered, and the method has a good practical value.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of phosphine palladium, and in particular relates to a preparation method of dichlorodi-tert-butyl-4-dimethylaminophenylphosphine palladium. Background technique [0002] Dichlorodi-tert-butyl-(4-dimethylaminophenyl)phosphine palladium plays an important role in the current practical application of organic synthesis. It is mainly used as a catalyst in C-C and C-N coupling reactions. It is used in chemical raw materials, It is widely used in the synthesis of liquid crystal monomer materials, optical functional materials and other substances. In the synthesis of these compounds, high-quality dichlorodi-tert-butyl-(4-dimethylaminophenyl)phosphine palladium has a very efficient catalytic effect. [0003] At present, in order to obtain high-quality dichlorodi-tert-butyl-(4-dimethylaminophenyl) phosphine palladium, many dichlorodi-tert-butyl-(4-dimethylaminophenyl) phosphine palladiums have...

Claims

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Application Information

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IPC IPC(8): C07F15/00
CPCC07F15/0066
Inventor 张文赵磊侯云集蔡万煜
Owner 陕西瑞科新材料股份有限公司
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