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Micro-reaction system and method for continuously preparing 2-methyl-4-amino-5-aminomethylpyrimidine by using same

A technology of aminomethylpyrimidine and micro-reaction, applied in chemical instruments and methods, chemical/physical/physicochemical reactors, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of low process efficiency, synthetic Short route, high reaction pressure and other problems, to achieve the effect of improving efficiency, time-space yield, small liquid holding capacity, and high space-time efficiency

Active Publication Date: 2021-02-09
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method raw material is easy to get and cheap, and the synthetic route of 2-methyl-4-amino-5-cyanopyrimidine is short, but outstanding shortcoming is that 2-methyl-4-amino-5-cyanopyrimidine catalytic hydrogenation Long reaction time, high reaction pressure, high risk, high energy consumption, and low process efficiency

Method used

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  • Micro-reaction system and method for continuously preparing 2-methyl-4-amino-5-aminomethylpyrimidine by using same
  • Micro-reaction system and method for continuously preparing 2-methyl-4-amino-5-aminomethylpyrimidine by using same
  • Micro-reaction system and method for continuously preparing 2-methyl-4-amino-5-aminomethylpyrimidine by using same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 1. Preparation of modified Raney nickel catalyst

[0061] Disperse 40 g of 20-40 mesh Raney nickel in 100 g of water, add 5% formalin solution of Raney nickel weight, stir at 25°C for 2 hours under nitrogen protection, then filter and wash with deionized water three times , that is, the modified Raney nickel catalyst is prepared, and finally stored in water.

[0062] 2. Catalytic hydrogenation reaction

[0063] The Raney nickel catalyst modified in this example above was filled in a tubular microchannel reactor (length 20 cm, inner diameter 1 cm). Take 5 g of ammonia water (25 wt.%) and 200 ml of methanol to prepare a methanol solution of ammonia water, then add 2-methyl-4-amino-5-cyanopyrimidine (2 g, 0.015 mol) to the above ammonia water Methanol solution was prepared as a substrate liquid, and then the substrate liquid and hydrogen gas were delivered to the T-type micro-mixer at the same time. The molar ratio of 2-methyl-4-amino-5-cyanopyrimidine to hydrogen is 1:...

Embodiment 2

[0065] This example is the same as Example 1, the only difference being that the preparation of the modified Raney nickel catalyst in this example is 60-80 mesh Raney nickel. In this example, the substrate 2-methyl-4-amino-5-cyanopyrimidine was completely converted, and the yield of the product 2-methyl-4-amino-5-aminomethylpyrimidine was 100%, and the purity was greater than 99%.

Embodiment 3

[0067] This example is the same as Example 2, the only difference is that in the catalytic hydrogenation reaction experiment in this example, the reaction of the mixed reaction material formed after the substrate liquid and hydrogen are mixed in a T-type micro-mixer in a microchannel reactor The time is about 1.2 minutes. In this example, the substrate 2-methyl-4-amino-5-cyanopyrimidine was completely converted, and the yield of the product 2-methyl-4-amino-5-aminomethylpyrimidine was 100%, and the purity was greater than 99%.

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Abstract

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.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical engineering, and in particular relates to a micro-reaction system and a method for continuously preparing 2-methyl-4-amino-5-aminomethylpyrimidine using the same. Background technique [0002] 2-Methyl-4-amino-5-aminomethylpyrimidine (I) is a synthetic vitamin B 1 important intermediates. [0003] [0004] US Patent 3689498, US Patent 3792076, US Patent 3853946, US Patent 3901888, US Patent 2820050, UK Patent 772256, German Patent 2323845 and Todd and Bergel ( J. Chem. Soc. , 1937, 364) etc. have described the method for preparing 2-methyl-4-amino-5-aminomethylpyrimidine by hydrolysis of 2-methyl-4-amino-5-acetylaminomethylpyrimidine. In this method, the synthesis route of 2-methyl-4-amino-5-acetylaminomethylpyrimidine is long, the process is complicated, the cost is high and the environment is polluted heavily, so it is difficult to be applied industrially. World patent WO2012 / 075677...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/42B01J8/06
CPCC07D239/42B01J8/06B01J8/065B01J19/0093B01J2219/00889B01J2219/00909B01J2219/00961B01J2219/00963B01J2219/00959B01J2219/00984B01J23/755B01J25/02
Inventor 陈芬儿姜梅芬程荡黄华山刘敏杰王路路
Owner FUDAN UNIV
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