Refining process of 5-methoxy-4, 6-dichloropyrimidine

A technology of dichloropyrimidine and methoxy, which is applied in the field of refining process of 5-methoxy-4,6-dichloropyrimidine, can solve the problems of low molding yield, high preparation cost, and no debugging process, etc. To achieve the effect of stable control ratio

Inactive Publication Date: 2020-08-04
CHANGSHU JINSHEN MEDICAL PROD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] When the existing 5-methoxy-4,6-dichloropyrimidine is prepared, the molding yield of its raw material preparation is low, which makes the preparation cost higher, and the finished product 5-methoxy-4,6-dichloropyrimidine The use stability of chloropyrimidine is poor, and it has not been well debugged, which is not conducive to the control of personnel preparation in the later stage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The refining process of 5-methoxy-4,6-dichloropyrimidine includes the following parts by weight of materials: 16 parts by weight of 2-methoxy-malonic acid dicarboxylic acid, 2.5 parts by weight of phosphorus oxychloride, and 5 parts by weight of methanol Parts, 3 parts by weight of sodium ethylate, 2 parts by weight of ethanol, 5 parts by weight of 2-methoxy-malonamide, 4 parts by weight of formamide, 1 part by weight of dichloromethane, 0.4 parts by weight of phosphorus oxychloride, N, 8.2 parts by weight of N-dimethylaniline, 2 parts by weight of trichloroethylene;

[0023] Concrete preparation process is as follows:

[0024] Step 1: Take 2 / 3 methanol and add 2-methoxy-malonic acid dicarboxylic acid to dissolve 2-methoxy-malonic acid dicarboxylic acid, then adjust the temperature to -1°C, and pass ammonia gas React it for 2 hours, wash it with 1 / 3 methanol after filtering, and then vacuum-dry it at a temperature of 41°C to obtain 2-methoxy-malonamide with a yield of ...

Embodiment 2

[0038] The refining process of 5-methoxy-4,6-dichloropyrimidine includes the production of the following materials in parts by weight: 16.5 parts by weight of 2-methoxy-malonic acid dicarboxylic acid, 3 parts by weight of phosphorus oxychloride, and 8 parts by weight of methanol Parts, 5 parts by weight of sodium ethylate, 3 parts by weight of ethanol, 6 parts by weight of 2-methoxy-malonamide, 5 parts by weight of formamide, 2 parts by weight of methylene chloride, 0.8 parts by weight of phosphorus oxychloride, N, 8.8 parts by weight of N-dimethylaniline, 3 parts by weight of trichloroethylene;

[0039] Concrete preparation process is as follows:

[0040] Step 1: Take 2 / 3 methanol and add 2-methoxy-malonic acid dicarboxylic acid to dissolve 2-methoxy-malonic acid dicarboxylic acid, then adjust the temperature to -0°C, and use ammonia gas to It was reacted for 4 hours, filtered, washed with 1 / 3 methanol, and then vacuum-dried at a temperature of 45°C to obtain 2-methoxy-malon...

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PUM

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Abstract

The invention discloses a preparation method of 5-methoxy-4, 5-dimethyl-1, 3-dioxolane. The preparation method comprises the following steps: adding 2 / 3 of methanol into 2-methoxy-malonic acid dicarboxylic acid; dissolving 2-methoxy-malonic acid dicarboxylic acid, adjusting the temperature to -1 DEG C to 0 DEG C, carrying out a reaction for 2-4 h with ammonia gas, filtering, washing with 1 / 3 methanol, and carrying out vacuum drying at 41-45 DEG C to obtain 2-methoxy-malonamide with a yield of 91-93%; heating and stirring sodium ethoxide, 2 / 3 of ethanol and the 2-methoxy-malonamide obtained inthe step 1; during stirring, stirring is conducted for 35-40 min at the temperature of 18-19 DEG C, adding formamide, performing a reflux reaction, adding 1 / 3 of ethyl alcohol for washing after filtering, performing vacuum drying treatment at the temperature of 51-55 DEG C, and obtaining 4, 6-dihydroxy-5-methoxypyrimidine disodium salt, wherein the yield reaches 87-89%. The molding yield of the 5-methoxy-4, 6-dichloropyrimidine preparation is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a refining process of 5-methoxy-4,6-dichloropyrimidine. Background technique [0002] When the existing 5-methoxy-4,6-dichloropyrimidine is prepared, the molding yield of its raw material preparation is low, which makes the preparation cost higher, and the finished product 5-methoxy-4,6-dichloropyrimidine The use stability of chloropyrimidine is poor, and it has not been well debugged, which is not conducive to the control of personnel preparation in the later stage. Contents of the invention [0003] The object of the present invention is to provide a refining process for 5-methoxy-4,6-dichloropyrimidine to solve the problems raised in the above-mentioned background technology. [0004] In order to achieve the above object, the present invention provides the following technical scheme: the refining process of 5-methoxy-4,6-dichloropyrimidine, including t...

Claims

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Application Information

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