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Process for preparing 2-methyl-4-amino-5-acetyl aminomethyl pyrimidine

A technology of acetamidomethazine and amino, applied in the direction of organic chemistry, etc., can solve the problems of difficult control of process conditions, low content of acetylpyrimidine, long process time, etc., and achieve easy control of process conditions, excellent quality, and avoid salt content The effect of wastewater

Active Publication Date: 2012-06-13
HUAZHONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method not only has a low yield, but also takes a long time to process, the process conditions are not easy to control, the content of acetylpyrimidine is low, and a large amount of high-concentration wastewater containing inorganic salts is produced in the production process.

Method used

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  • Process for preparing 2-methyl-4-amino-5-acetyl aminomethyl pyrimidine
  • Process for preparing 2-methyl-4-amino-5-acetyl aminomethyl pyrimidine
  • Process for preparing 2-methyl-4-amino-5-acetyl aminomethyl pyrimidine

Examples

Experimental program
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Effect test

example 1

[0017] Example 1. With the methanol solution of 100 grams of 28% sodium methylate, 300g acetamidine hydrochloride (93%, 2.951mol), drop in the dry three-necked flask of 500ml band stirring, stir reaction 3 hours, filter desalting, the free The liquid was warmed up, and the filtrate was concentrated under reduced pressure to make the concentration of acetamidine reach 30%. Put the concentrated solution and 350g acetal (95%, 2.089mol) into a 1000ml dry three-necked flask with stirring, react at 20~25°C for 2 hours, dry formazan and ethanol under reduced pressure, and then add 200g pure water into the three-necked flask , heat up to 70°C, recover the low boiling point under vacuum, then heat up to 90°C for 30 minutes and then hydrolyze it for 30 minutes, add 600g of absolute ethanol, cool down to 0°C, filter to obtain 98.9% purity Product 247.4 g. The ethanol in the filtered mother liquor was recovered, and 28.3 grams of acetamidomethylpyrimidine with a content of 96.0% was obta...

example 2

[0018] Example 2. The operation is the same as in Example 1. 100 grams of 28% sodium methylate, 300g acetamidine hydrochloride (93%, 2.951mol), stirred and reacted for 3 hours, filtered to desalinate, and concentrated the filtrate under reduced pressure to obtain the concentration of 80% acetamidine concentration Liquid and 350g acetal (95%, 2.089mol) reacted for 2 hours at 25~28°C, dried methyl alcohol under reduced pressure, then added 200g pure water into the three-necked flask, raised the temperature to 70°C, recovered the low boiling point in vacuum, and then After heating up to 90°C for 30 minutes for hydrolysis, methanol was added, the temperature was lowered to 0°C, and 266.2 g of a finished product with a purity of 98.0% was obtained by filtration. The ethanol in the filtered mother liquor was recovered, and 30.0 g of acetamidomethylpyrimidine with a content of 95.0% was obtained simultaneously.

[0019] Example 3. According to the method for example 1, the acetamidin...

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Abstract

The invention discloses a preparation method of 2-methyl-4-amino-5-acetylaminomethyl pyrimidine. The preparation method is characterized in that acetamidine hydrochloride reacts with sodium methoxide or sodium alcoholate to obtain alcoholic solution of ethanamidine after removing generated sodium chloride by filtration, and ethanamidine solution with a certain concentration is obtained after concentration; the ethanamidine solution react with acetal, methanol or ethanol is depressurized to dryness, then an obtained resultant is hydrolyzed to obtain crude acetylpyrimidine, and fixed amount of methanol or ethanol solution is added to separate refined acetylpyrimidine by crystallization. The methanol or the ethanol can be recovered from crystallization mother liquor in a distillation way, the recovered methanol or the ethanol can be applied to next batch, distillation residue is cooled and filtered after being added with a little water, and the acetylpyrimidine dissolved in a solvent is recovered. The preparation method has the advantages of high yield, good quality of the obtained product, no environmental pollution and the like.

Description

Technical field: [0001] The invention relates to a preparation method of vitamin B1 intermediate 2-methyl-4-amino-5-acetylaminomethylpyrimidine. Background technique: [0002] The industrial synthesis method of known 2-methyl-4-amino-5 acetylaminomethylpyrimidine (hereinafter referred to as acetylpyrimidine) is as follows: [0003] [0004] This reaction generates formazan, ethanol and a large amount of sodium chloride while generating the target product acetylpyrimidine. The mixing of sodium chloride and acetylpyrimidine not only affects the progress of the reaction, but also requires a large amount of water crystallization to remove the sodium chloride therein. , The process conditions in industrial production are not easy to control, the content of acetylpyrimidine is low, and a large amount of high-concentration wastewater containing inorganic salts is produced in the production process. [0005] 2-methyl-4-amino-5-acetylaminomethylpyrimidine (I) is an important inte...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/42
Inventor 王勇付林魏旭力徐勇陈胜红
Owner HUAZHONG PHARMA
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