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The preparation method of 5-methoxy-4,6-dichloropyrimidine

A technology of dichloropyrimidine and methoxy, which is applied in the field of preparation of 5-methoxy-4,6-dichloropyrimidine, can solve the problem of low yield and achieve the effect of high yield

Active Publication Date: 2017-01-11
CHANGSHU JINSHEN MEDICAL PROD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The existing preparation method of 5-methoxy-4,6-dichloropyrimidine has low yield

Method used

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Examples

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Embodiment Construction

[0010] The specific implementation of the present invention will be further described below in conjunction with the examples. The following examples are only used to illustrate the technical solution of the present invention more clearly, but not to limit the protection scope of the present invention.

[0011] The technical scheme of concrete implementation of the present invention is:

[0012] A preparation method of 5-methoxy-4,6-dichloropyrimidine, comprising the steps of:

[0013] 1) Put 31 parts by mass of 5-methoxy-4,6-dihydroxypyrimidine disodium and 42 parts by mass of phosphorus oxychloride into the reactor, keep it warm at 65°C for 1.5 hours, and recover phosphorus oxychloride under reduced pressure until the material is dry ;

[0014] 2) Cool to 35°C, add trichlorethylene, put it into a hydrolysis pot, then add 650 parts by mass of water, and stir at 65°C;

[0015] 3) Remove the trichlorethylene layer, add trichlorethylene, repeat extraction 9 times, put the tric...

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PUM

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Abstract

The invention discloses a preparation method of 5-methoxyl-4,6-dichloro pyrimidine. The method includes the steps of firstly, adding 31 parts of 5-methoxyl-4,6-dihydroxy pyrimidine disodium and 42 parts of phosphorus oxychloride into a reaction kettle, keeping the temperature at 65 DEG C for 1.5 hours, and reducing pressure to recycle phosphorus oxychloride until the material is dried; secondly, cooling to 35 DEG C, adding trichloro ethylene, placing into a hydrolysis pot, adding 650 parts of water, and stirring at 65 DEG C; thirdly, removing the trichloro ethylene layer, adding the trichloro ethylene again, repeatedly extracting for 9 times, and placing the trichloro ethylene layer into a distillatory kettle to recycle the trichloro ethylene so as to obtain coarse chloride; fourthly, adding the coarse chloride into a refining kettle, adding methanol three times as much as the coarse chloride, heating to achieve full dissolution, cooling to 45 DEG C, and discharging and drying to obtain 19 parts of 5-methoxyl-4,6-dichloro pyrimidine. The method is high in 5-methoxyl-4,6-dichloro pyrimidine yield.

Description

technical field [0001] The invention relates to a preparation method of 5-methoxy-4,6-dichloropyrimidine. Background technique [0002] The existing preparation method of 5-methoxy-4,6-dichloropyrimidine has low yield. Contents of the invention [0003] The purpose of the present invention is to provide a method for preparing 5-methoxy-4,6-dichloropyrimidine, which has a high yield of 5-methoxy-4,6-dichloropyrimidine. [0004] In order to achieve the above object, the technical solution of the present invention is to design a preparation method of 5-methoxy-4,6-dichloropyrimidine, comprising the steps of: [0005] 1) Put 31 parts by mass of 5-methoxy-4,6-dihydroxypyrimidine disodium and 42 parts by mass of phosphorus oxychloride into the reactor, keep it warm at 65°C for 1.5 hours, and recover phosphorus oxychloride under reduced pressure until the material is dry ; [0006] 2) Cool to 35°C, add trichlorethylene, put it into a hydrolysis pot, then add 650 parts by mass ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/34
CPCC07D239/34
Inventor 李涛
Owner CHANGSHU JINSHEN MEDICAL PROD CO LTD
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