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Method for preparing 2-chloropyrimidine-4 formic acid

A technology of chloropyrimidine and methylpyrimidine hydrochloride, applied in the field of compound synthesis

Inactive Publication Date: 2016-11-09
安徽沛成医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is no report about the synthesis of 2-chloropyrimidine-4 formic acid at present, so it is necessary to provide a method for preparing 2-chloropyrimidine-4 formic acid

Method used

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  • Method for preparing 2-chloropyrimidine-4 formic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 4.09kg of phosphorus oxychloride and 1.6Kg of raw material A to a 10L reaction bottle, heat to 80 degrees; add 2.22kg of triethylamine dropwise (slow and easy to block), turn off the heating, and maintain the temperature by exothermic reaction ; After dripping, react at 100-105°C for 4h, monitored by TLC. After the reaction, the temperature was lowered to 30° C. for post-treatment.

[0018] Post-treatment: slowly pour the reaction solution into 40L of crushed ice to decompose phosphorus oxychloride; add 2L of dichloroethane to disperse the reaction system to facilitate pouring out the material, and then adjust the pH to 6-7 with 30% sodium hydroxide; Add 4L of ethyl acetate to extract 3 times, combine the extracted and separated organic phases, decolorize with dry activated carbon, filter with suction, and spin dry to obtain 970g of reddish-brown solid product. Test results: melting point around 45 degrees, HPLC: 220nm, 60:40, 97.6% theory: 1403g, yield: 69.1%.

...

Embodiment 2

[0024] Add 4.09kg of phosphorus oxychloride and 1.6Kg of raw material A to a 10L reaction bottle, heat to 80 degrees; add 2.22kg of triethylamine dropwise (slow and easy to block), turn off the heating, and maintain the temperature by exothermic reaction ; After dripping, react at 100-105°C for 4h, monitored by TLC. After the reaction, the temperature was lowered to 30° C. for post-treatment.

[0025] Post-treatment: slowly pour the reaction solution into 40L of crushed ice to decompose phosphorus oxychloride; add 2L of dichloroethane to disperse the reaction system to facilitate pouring out the material, and then adjust the pH to 6-7 with 30% sodium hydroxide; Add 4L of ethyl acetate to extract 3 times, combine the extracted and separated organic phases, decolorize with dry activated carbon, filter with suction, and spin dry to obtain 970g of reddish-brown solid product. Test results: melting point around 45 degrees, HPLC: 220nm, 60:40, 97.6% theory: 1403g, yield: 69.1%.

...

Embodiment 3

[0031] Combine the concentrated and dried products in Example 1 and Example 2, add 3L*2 times of methanol to reflux to extract the product, concentrate the methanol to semi-dryness, cool and filter to obtain 250g of the product, and concentrate and dry the mother liquor to obtain 60g of the crude product, with a yield of 44%. The spectrum of the measured product is as figure 1 shown.

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Abstract

The invention relates to a method for preparing 2-chloropyrimidine-4 formic acid. The method comprises the following steps: performing debydrochlorination reaction on 2-chlorine-4-methyl pyridine hydrochloride and phosphorus oxychloride and separating, thereby acquiring 2-chlorine-4-methyl pyridine; and performing methyl oxidizing reaction on 2-chlorine-4-methyl pyridine and methyl oxidant and separating, thereby acquiring 2-chloropyrimidine-4 formic acid. According to the process route provided by the invention, the yield of the target product is high, the process route can be amplified, the raw materials can be easily acquired and have low cost, and industrial production can be carried out.

Description

technical field [0001] The invention relates to the field of compound synthesis, in particular to a method for preparing 2-chloropyrimidine-4carboxylic acid. Background technique [0002] 2-Chloropyrimidine-4-carboxylic acid can be used as a key intermediate in the treatment of hyperphosphatemia and in the synthesis of benzenesulfonamide pyrazole kinase inhibitors. But there is no report about the synthesis of 2-chloropyrimidine-4 formic acid, so it is necessary to provide a method for preparing 2-chloropyrimidine-4 formic acid. Contents of the invention [0003] The object of the present invention is to provide a method for preparing 2-chloropyrimidine-4 formic acid, which can effectively prepare 2-chloropyrimidine-4 formic acid and provide a basis for industrial production. [0004] To achieve the above object, the present invention adopts the following technical solutions: [0005] A method for preparing 2-chloropyrimidine-4 formic acid, comprising the following opera...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/30
CPCC07D239/30
Inventor 魏晓延贺鹰魏巍余利灯
Owner 安徽沛成医药科技有限公司
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