Synthesis process of 2-chloropyrimidin

A synthesis process, a technology of chloropyrimidine, which is applied in the field of synthesis process for preparing 2-chloropyrimidine, can solve the problems of low product purity and low yield

Inactive Publication Date: 2015-07-08
TAICANG YUNTONG BIOCHEM ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the prior art, the synthesis process of 2-chloropyrimid...

Method used

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  • Synthesis process of 2-chloropyrimidin
  • Synthesis process of 2-chloropyrimidin
  • Synthesis process of 2-chloropyrimidin

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Add absolute ethanol and 1.2mol guanidine nitrate into a 250ml four-necked flask, continuously feed dry hydrogen chloride gas into the absolute ethanol and keep stirring, and after adjusting the temperature to 10-20°C, add 1 mol of 1,1,3,3-tetramethoxypropane, the temperature of the reaction system was stabilized at 20°C, and the cyclization reaction was carried out for 6 hours. After the reaction is complete, collect the formed precipitate by filtration, add the precipitate into water and add sodium hydroxide solution to adjust the pH to 9, add toluene for dehydration and separate the clear liquid while it is hot, extract the solid with toluene, combine the organic phases, and filter by cold analysis. The fine product 2-aminopyrimidine was obtained.

[0016] Add 2.5mol of hydrochloric acid and 80g of dichloromethane into a 500mL reactor, and then add 1mol of 2-aminopyrimidine under stirring. Add 3.2mol ZnCl at 10~15℃ 2 , After reacting for 30min, a dark yellow suspen...

Embodiment 2

[0018] Add absolute ethanol and 1.8mol guanidine nitrate to a 250ml four-necked flask, continuously feed dry hydrogen chloride gas into the absolute ethanol and keep stirring, and after adjusting the temperature to 10-20°C, add 1 mol of 1,1,3,3-tetramethoxypropane, the temperature of the reaction system was stabilized at 30°C, and the cyclization reaction was carried out for 4 hours. After the reaction is completed, collect the formed precipitate by filtration, add the precipitate to water and add sodium hydroxide solution to adjust the pH to 10, add toluene for dehydration, separate the clear liquid while hot, extract the solid with toluene, combine the organic phases, and filter by cold analysis. The fine product 2-aminopyrimidine was obtained.

[0019] Add 3.5mol of hydrochloric acid and 80g of dichloromethane into a 500mL reactor, and then add 1mol of 2-aminopyrimidine under stirring. Add 4mol ZnCl at 10~15℃ 2 , After reacting for 60min, a dark yellow suspension was gene...

Embodiment 3

[0021] Add absolute ethanol and 1.5mol guanidine nitrate into a 250ml four-necked flask, continuously feed dry hydrogen chloride gas into the absolute ethanol and keep stirring, and after adjusting the temperature to 10-20°C, add 1 mol of 1,1,3,3-tetramethoxypropane, the temperature of the reaction system was stabilized at 25°C, and the cyclization reaction was carried out for 5 hours. After the reaction is complete, collect the formed precipitate by filtration, add the precipitate to water and add sodium hydroxide solution to adjust the pH to 9.5, add toluene for dehydration, separate the clear liquid while hot, extract the solid with toluene, combine the organic phases, and filter by cold analysis. The fine product 2-aminopyrimidine was obtained.

[0022] Add 3 mol of hydrochloric acid and 80 g of dichloromethane into a 500 mL reactor, and then add 1 mol of 2-aminopyrimidine under stirring. Add 3.5mol ZnCl at 10~15℃ 2 , After reacting for 45min, a dark yellow suspension wa...

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Abstract

The invention discloses a synthesis process of 2-chloropyrimidine. The synthesis method of the invention is as below: reacting guanidine nitrate and 1,1,3,3-tetramethoxy propane in an absolute ethyl alcohol solvent with continuous introduction of dry hydrogen chloride gas at 20-30 DEG C for 4-6 h to obtain 2-aminopyrimidine; and then reducing 2-aminopyrimidine in the presence of catalysts of NaNO2, HCl and ZnCl2 at -10-5 DEG C to obtain the product. Through the above preparation route, 2-chloropyrimidine with high purity and high yield can be obtained.

Description

technical field [0001] The invention relates to the technical field of 2-chloropyrimidine preparation, in particular to a synthesis process 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 synthesis process of 2-chloropyrimidine in the prior art has the technical defects of low yield and low product purity. Contents of the invention [0003] In view of this, the present invention provides a process for preparing 2-chloropyrimidine, the product of the preparation process has higher purity and higher yield. [0004] A kind of synthetic technique of 2-chloropyrimidine, comprises the following steps: [0005] (1) Put guanidine nitrate (formula A) and 1,1,3,3-tetramethoxypr...

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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