Method of preparing 2-chloropyrimidine

A chloropyrimidine and reaction technology, applied in the field of 2-chloropyrimidine preparation, can solve the problems of low product purity and low yield, and achieve the effects of high purity and high yield

Inactive Publication Date: 2015-03-04
TAICANG YUNTONG BIOCHEM ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method for preparing 2-chloropyrimidine in the prior art has technical defects that the yield of the substance is low and the product purity is low

Method used

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  • Method of preparing 2-chloropyrimidine
  • Method of preparing 2-chloropyrimidine
  • Method of preparing 2-chloropyrimidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 1.05mol urea and 25wt% methanol solution of sodium methoxide (1.15mol in methanol) into a 1000mL four-neck bottle, slowly add 1mol diethyl malonate dropwise at reflux temperature, stir and reflux for 2 hours, and obtain a large amount of white powder The solid was concentrated under reduced pressure to obtain a white sodium salt dry powder, to which was added 38 wt% dilute hydrochloric acid solution, water was added to adjust the pH to 1.5, heated to 65°C, and allowed to react for 4 hours. After the reaction was completed, the temperature was lowered to 0° C. to precipitate crystals, and the crystals were filtered out. Recrystallize from a methanol / water mixed solution to obtain a white powder, which is the product barbituric acid.

[0020] Put 5.1mol phosphorus oxychloride and N,N-dimethylaniline (60mL) into a 1000mL four-neck bottle, heat to 40°C, add barbituric acid in batches within 30-60min, and keep the temperature at 40°C . After adding the barbituric acid,...

Embodiment 2

[0023] Put 1.15mol of urea and 25wt% methanol solution of sodium methoxide into a 1000mL four-necked bottle (the methanol contains 1.25mol), slowly add 1mol of diethyl malonate dropwise at reflux temperature, stir and reflux for 3 hours, and obtain a large amount of white powder The solid was concentrated under reduced pressure to obtain a white sodium salt dry powder, to which was added 38wt% dilute hydrochloric acid solution, water was added to adjust the pH to 3, and heated to 75°C for 2 hours to react. After the reaction was completed, the temperature was lowered to 0° C. to precipitate crystals, and the crystals were filtered out. Recrystallize from a methanol / water mixed solution to obtain a white powder, which is the product barbituric acid.

[0024] Put 5.5mol phosphorus oxychloride and N,N-dimethylaniline (60mL) into a 1000mL four-necked bottle, heat to 40°C, add barbituric acid in batches within 30-60min, and keep the temperature at 50°C . After adding the barbitur...

Embodiment 3

[0027] Put 1.10mol of urea, 25wt% sodium methoxide (), methanol solution (1.20mol in methanol) into a 1000mL four-necked bottle, slowly add 1mol of diethyl malonate dropwise at reflux temperature, stir and reflux for 2 hours, and obtain a large amount of white The powdery solid was concentrated under reduced pressure to obtain a white sodium salt dry powder, to which was added 38 wt% dilute hydrochloric acid solution, water was added to adjust the pH to 2.5, heated to 65-75°C, and allowed to react for 3 hours. After the reaction was completed, the temperature was lowered to 0° C. to precipitate crystals, and the crystals were filtered out. Recrystallize from a methanol / water mixed solution to obtain a white powder, which is the product barbituric acid.

[0028] Put 5.3mol phosphorus oxychloride and N,N-dimethylaniline (60mL) into a 1000mL four-necked bottle, heat to 40°C, add barbituric acid in batches within 30-60min, and keep the temperature at 45°C . After adding the barb...

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Abstract

The invention discloses a method of preparing 2-chloropyrimidine. The method comprises the following steps: firstly carrying out reaction on malonic acid bis-ethylacetate and urea with sodium methoxide as a catalyst to obtain barbituric acid, then carrying out reaction on the barbituric acid and phosphorus oxychloride with N, N-dimethylaniline as a catalyst to obtain 2, 4, 6-trichloropyrimidine, and finally carrying out redox reaction on the 2, 4, 6-trichloropyrimidine and zinc powder in a solvent of methanol and water under the alkaline condition to obtain the 2-chloropyrimidine, wherein the molar ratio of the 2, 4, 6-trichloropyrimidine to the zinc powder is 1:(1-1.2). According to the method disclosed by the invention, by virtue of the 2, 4, 6-trichloropyrimidine and the zinc powder with the molar ratio to be 1:(1-1.2), only chlorine on 4 and 6 bits on a pyrimidine ring of the 2, 4, 6-trichloropyrimidine can be reduced, so that the side effect of generating dichloride or pyrimidine is reduced; and by virtue of the reaction route, the 2-chloropyrimidine with high purity and yield is obtained.

Description

technical field [0001] The invention relates to the technical field of 2-chloropyrimidine preparation, in particular to a method for preparing 2-chloropyrimidine. Background technique [0002] 2-Chloropyrimidine, also known as 2-chloropyridoline, has a molecular formula of C 4 h 3 ClN 2 , its molecular weight is 114.53, and its CAS number is 1722-12-9. It is a white or light yellow powder with a melting point of 63-66°C, a boiling point of 75-76°C and a flash point of 98°C. The method for preparing 2-chloropyrimidine in the prior art has technical defects of low yield and low product purity. Contents of the invention [0003] In view of this, the present invention provides a method for preparing 2-chloropyrimidine, the product of the preparation method has higher purity and higher yield. [0004] A method for preparing 2-chloropyrimidine, comprising the following steps: [0005] (1) Ethyl malonate diacetate and urea are reacted under the condition of using sodium meth...

Claims

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Application Information

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IPC IPC(8): C07D239/30
CPCC07D239/30
Inventor 张卫东
Owner TAICANG YUNTONG BIOCHEM ENG
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