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The preparation method of 2-methyl-4-amino-5-(aminomethyl)pyrimidine

A technology of aminomethyl and amino, which is applied in the field of preparation of intermediates, can solve the problems of environmental protection, a large amount of salt, and uneconomical waste liquid, and achieve the effect of simple operation

Active Publication Date: 2016-04-27
江西天新药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to overcome the defects that a large amount of salts and waste liquid are uneconomical and not environmentally friendly in the existing preparation method of 2-methyl-4-amino-5-(aminomethyl)pyrimidine, and provide an economical, Preparation method of 2-methyl-4-amino-5-(aminomethyl)pyrimidine which is environment-friendly and suitable for industrialized production

Method used

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  • The preparation method of 2-methyl-4-amino-5-(aminomethyl)pyrimidine

Examples

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preparation example Construction

[0012] The invention provides a method for preparing 2-methyl-4-amino-5-(aminomethyl)pyrimidine, wherein the method comprises: in the presence of an alkali agent, 2-methyl-4-amino-5 -(formamidomethyl)pyrimidine and methanol carry out a contact reaction, the weight ratio of the amount of the alkaline agent to the amount of the 2-methyl-4-amino-5-(formamidomethyl)pyrimidine is 0.001-0.05 :1.

[0013] According to the method provided by the present invention, the amount of 2-methyl-4-amino-5-(carboxamidomethyl)pyrimidine and methanol is not particularly limited, preferably, the 2-methyl-4- The molar ratio of the amount of amino-5-(formamidomethyl)pyrimidine to the amount of methanol is 1:1-100, further preferably, the 2-methyl-4-amino-5-(formamide The molar ratio of methyl)pyrimidine to the methanol is 1:20-40.

[0014] According to the method provided by the invention, the alkaline agent is used to catalyze the reaction of 2-methyl-4-amino-5-(carboxamidomethyl) pyrimidine and ...

Embodiment 1

[0032] Add 100g of 2-methyl-4-amino-5-(carboxamidomethyl)pyrimidine obtained in the preparation example, 720ml of methanol and 2g of sodium methoxide into a 1000ml autoclave, start stirring, and keep the reaction at 100°C for 8h. Then the reaction mixture was cooled to 50°C, suction filtered, and the filtrate obtained by suction filtration was transferred to a three-necked flask for atmospheric distillation and concentration to obtain 23ml of methyl formate and recover 635ml of methanol. The concentrated residue was vacuum-dried at a vacuum degree of 0.05 MPa and a temperature of 80° C. for 3 hours to obtain 61.9 g of a light yellow solid. The content of 2-methyl-4-amino-5-(aminomethyl)pyrimidine detected by HPLC was 99.6%.

Embodiment 2

[0034] Add 100g of 2-methyl-4-amino-5-(carboxamidomethyl)pyrimidine obtained in the preparation example, 482ml of methanol and 1g of sodium methoxide into a 1000ml autoclave, start stirring, and keep the reaction at 120°C for 2h. Then the reaction mixture was cooled to 25°C, suction filtered, and the filtrate obtained by suction filtration was transferred to a three-necked flask for atmospheric distillation and concentration to obtain 21 ml of methyl formate and recover 392 ml of methanol. The concentrated residue was vacuum-dried at a vacuum degree of 0.09 MPa and a temperature of 50° C. for 5 hours to obtain 58.2 g of a light yellow solid. The content of 2-methyl-4-amino-5-(aminomethyl)pyrimidine detected by HPLC was 99.2%.

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Abstract

The invention discloses a preparation method of 2-methyl-4-amino-5-(aminomethyl) pyrimidine. The preparation method is characterized by comprising the following steps: in the presence of an alkaline agent, contacting 2-methyl-4-amino-5-(formamide methyl) pyrimidine with methanol to react, wherein the weight ratio of the amount of the alkaline agent to the amount of the 2-methyl-4-amino-5-(formamide methyl) pyrimidine is (0.001-0.05) to 1. According to the method provided by the invention, a great deal of organic salts, inorganic salts and liquid waste are not produced, and byproducts as well as the residual methanol can be completely recycled. The preparation method is economical, environmentally friendly and capable of meeting the development requirements of the existing national energy-saving environmental-protection industrial economy. Besides, the preparation method provided by the invention is simple to operate, easily available in raw material and suitable for the requirements of the industrial production. Moreover, the product is easy to separate and purify.

Description

technical field [0001] The invention relates to a preparation method of a vitamin B1 intermediate, in particular to a preparation method of 2-methyl-4-amino-5-(aminomethyl)pyrimidine. Background technique [0002] As an important basic nutrient component, vitamin B1 has a variety of important physiological functions, and its preparation method has attracted much attention. 2-Methyl-4-amino-5-(aminomethyl)pyrimidine (GDA) has also received extensive attention as a key intermediate for the preparation of vitamin B1. Its English name is: 2-methyl-4-amino- 5-(aminomethyl)pyrimidine, its structural formula is as follows: [0003] [0004] At present, with the efforts of chemists at home and abroad, a variety of routes for chemically synthesizing vitamin B1 have been formed. Among them, the process of preferentially synthesizing GDA, a key intermediate, has also been proved to be the most economical and effective. The production enterprises all adopt the method of finally pre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/42
CPCY02P20/582
Inventor 章根宝司玉贵郭军万真
Owner 江西天新药业股份有限公司