95-02-3Relevant articles and documents
Micro-reaction system and method for continuously preparing 2-methyl-4-amino-5-aminomethylpyrimidine by using same
-
Paragraph 0023-0055, (2021/02/10)
The invention belongs to the technical field of pharmaceutical engineering, and particularly relates to a micro-reaction system and a method for continuously preparing 2-methyl-4-amino-5-aminomethylpyrimidine by using the micro-reaction system. The method comprises the following steps: modifying a Raney nickel catalyst by using formalin, filling a micro-channel reactor with the modified Raney nickel catalyst; simultaneously conveying hydrogen and a substrate solution containing both 2-methyl-4-amino-5-cyanopyrimidine and an alkaline agent into the micro-reaction system comprising a micro-mixerand the micro-channel reactor which communicate with each other in sequence; and carrying out a continuous catalytic hydrogenation reaction to obtain the 2-methyl-4-amino-5-aminomethylpyrimidine. Compared with the prior art, the method provided by the invention has the advantages that reaction time is only several minutes, the yield of the product 2-methyl-4-amino-5-aminomethylpyrimidine is greater than 99%, a technological process is continuous, an automation degree is high, space-time yield is high, operation is simple and convenient, the separation steps of reaction liquid and a catalyst is not needed, cost is low, and industrial production is easy.
Fully continuous flow preparation method of 2-methyl-4-amino-5-aminomethylpyrimidine
-
Paragraph 0006; 0045; 0047-0061, (2021/07/17)
The invention discloses a fully continuous flow preparation method of 2-methyl-4-amino-5-aminomethylpyrimidine. The method comprises the following steps: mixing a mixed solution of cyanoacetamide, N, N-dimethylformamide and a catalyst with phosphorus oxychloride in a micro-mixer, and carrying out a continuous flow reaction in a micro-channel reactor to obtain (dimethyl aminomethylene) malononitrile; continuously quenching, continuously extracting and separating, concentrating an organic solution, mixing with a methanol solution, and continuously reacting with organic alkali to obtain 2-methyl-4-amino-5-cyanopyrimidine; continuously filtering the reaction mixed solution, dissolving the solid with methanol, conveying the dissolved solid and hydrogen to a fixed bed microchannel reactor through a micromixer, carrying out hydrogenation reaction, and concentrating, drying and purifying the product to obtain the 2-methyl-4-amino-5-aminomethylpyrimidine product. The method is mild in reaction condition, short in reaction time, high in product yield, low in energy consumption, green, safe and easy to industrially amplify and apply.
2-methyl-4-amino-5 - (aminomethyl) method for the preparation of pyrimidine
-
Paragraph 0031-0032, (2017/03/14)
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.