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Preparation process of 2-methyl-4-amino-5-pyrimidinemethanamine

A technology for the preparation of aminomethylpyrimidine, which is applied in the field of preparation of 2-methyl-4-amino-5-aminomethylpyrimidine, can solve the problems of low yield and lengthy route, and achieve high product yield, Low raw material cost and low pollution effect

Inactive Publication Date: 2019-02-01
NANJING JINHAO MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved in the present invention is to overcome the shortcomings of long and tedious synthetic method routes and low yields of 2-methyl-4-amino-5-aminomethylpyrimidine in the prior art, and to provide a

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] A preparation process of 2-methyl-4-amino-5-aminomethylpyrimidine, comprising the following steps:

[0018] 1) Add 27 parts of DMF and 48 parts of dimethyl sulfate into a four-necked flask, raise the temperature to 60°C, heat and stir for 3-6 hours, and then cool to 0°C;

[0019] 2), slowly add 48 parts of sodium methoxide methanol solution, after dropping, keep stirring for 10 minutes;

[0020] 3) Slowly add 27 parts of 3-aminopropionitrile, stir for 30 minutes, and distill under reduced pressure to obtain intermediate 1;

[0021] 4), then add 130 parts of dichloromethane and stir for 10 minutes, filter, and carry out vacuum distillation on the filtrate to obtain intermediate 2;

[0022] 5) Add 74 parts of sodium methoxide methanol solution into a four-neck flask, cool down to -5°C, slowly add 38 parts of acetamidine hydrochloride, keep stirring for 20 minutes, filter, transfer the filtrate to another flask and add intermediate 2 and 38 parts of sodium hydroxide, hea...

Embodiment 2

[0024] A preparation process of 2-methyl-4-amino-5-aminomethylpyrimidine, comprising the following steps:

[0025] 1) Add 1 part of DMF and 51 parts of dimethyl sulfate into a four-neck flask, heat up to 90°C, keep stirring for 6 hours, then cool to -15°C;

[0026] 2), slowly add 51 parts of sodium methoxide methanol solution, after dropping, keep stirring for 15 minutes;

[0027] 3) Slowly add 30 parts of 3-aminopropionitrile, stir for 60 minutes, and distill under reduced pressure to obtain intermediate 1;

[0028] 4), then add 150 parts of dichloromethane and stir for 30 minutes, filter, and carry out vacuum distillation on the filtrate to obtain intermediate 2;

[0029] 5) Add 77 parts of sodium methoxide methanol solution into a four-necked flask, cool down to 5°C, slowly add 41 parts of acetamidine hydrochloride, keep stirring for 40 minutes, filter, transfer the filtrate to another flask and add intermediate 2 and and 41 parts of sodium hydroxide, heated to 30°C, and ...

Embodiment 3

[0031] A preparation process of 2-methyl-4-amino-5-aminomethylpyrimidine, comprising the following steps:

[0032] 1) Add 30 parts of DMF and 50 parts of dimethyl sulfate into a four-neck flask, raise the temperature to 75°C, heat and stir for 4 hours, then cool to -10°C;

[0033] 2), slowly add 50 parts of sodium methoxide methanol solution, after dropping, keep stirring for 10 minutes;

[0034] 3) Slowly add 28 parts of 3-aminopropionitrile, stir for 40 minutes, and distill under reduced pressure to obtain intermediate 1;

[0035] 4), then add 140 parts of dichloromethane and stir for 20 minutes, filter, and carry out vacuum distillation on the filtrate to obtain intermediate 2;

[0036] 5) Add 75 parts of sodium methoxide methanol solution into a four-neck flask, cool down to -4°C, slowly add 40 parts of acetamidine hydrochloride, keep stirring for 30 minutes, filter, transfer the filtrate to another flask and add intermediate 2 and 40 parts of sodium hydroxide, heated to...

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Abstract

The invention discloses a preparation process of 2-methyl-4-amino-5-pyrimidinemethanamine. The preparation process of 2-methyl-4-amino-5-pyrimidinemethanamine comprises the following steps: 1) adding27-30 parts of DMF and 48-51 parts of dimethyl sulfate in a four-necked flask, heating to the temperature of 60-90 DEG C, insulating and stirring for 3-6 h, and then cooling; 2) adding 48-51 parts ofa methanol solution of sodium methylate, and after dropwise adding is finished, insulating and stirring for 5-15 min; 3) adding 27-30 parts of 3-aminopropionitrile, stirring for 30-60 min, and distilling under reduced pressure to obtain an intermediate 1; 4) then adding 130-150 parts of dichloromethane and stirring for 10-30 min, filtering, and distilling under reduced pressure to obtain an intermediate 2; and 5) adding 74-77 parts of a methanol solution of sodium methylate in the four-necked flask, cooling to the temperature of minus 5-5 DEG C, slowly adding 38-41 parts of acetamidine hydrochloride, insulating and stirring for 20-40 min, filtering, transferring to another flask and adding the intermediate 2 and 38-41 parts of NaOH, and stirring for 12-18 h after heating to obtain the final product. The preparation process of 2-methyl-4-amino-5-pyrimidinemethanamine is simple, and is low in pollution and low in raw material cost, and the yield of the product reaches up to 92.5%.

Description

technical field [0001] The invention relates to a preparation process of 2-methyl-4-amino-5-aminomethylpyrimidine. Background technique [0002] 2-methyl-4-amino-5-aminomethylpyrimidine is an important intermediate in the synthesis of vitamin B1 (Vitamin B1) and so on. The reported preparation methods of this compound mainly include the synthesis method using malonic acid derivatives as the starting material, the synthesis method using 3-(dimethylamino)propionitrile as the starting material, and the synthesis method using N,N-di A method for synthesizing methylformamide diethyl acetal as a starting material. The synthesis method has lengthy route, low yield and serious environmental pollution. Contents of the invention [0003] The technical problem to be solved by the present invention is to overcome the defects of lengthy route and low yield in the synthesis method of 2-methyl-4-amino-5-aminomethylpyrimidine in the prior art, and provide a method. [0004] In order to...

Claims

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Application Information

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IPC IPC(8): C07D239/42
CPCC07D239/42
Inventor 吴建中刘伟强童何兵蒋利华王步成
Owner NANJING JINHAO MEDICAL TECH CO LTD
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