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Method for purifying aminopyrimidine

A technology of aminopyrimidine and purification method, which is applied in the field of aminopyrimidine purification, and can solve the problems of low yield and quality of vitamin B1

Active Publication Date: 2019-03-22
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing process, the yield and quality of vitamin B1 synthesis are low

Method used

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  • Method for purifying aminopyrimidine
  • Method for purifying aminopyrimidine
  • Method for purifying aminopyrimidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A method for purifying aminopyrimidine, the steps of which are:

[0041] a. Formylpyrimidine: sodium hydroxide: water = 1:2:4 ratio, heat up and dissolve, keep warm at 100°C for 3 hours to obtain aminopyrimidine solution;

[0042] b. Cool down to 5-10°C, the aminopyrimidine solid precipitates out, and the aminopyrimidine is filtered out;

[0043] c. Wash the aminopyrimidine solid with methanol to remove impurities, and the ratio of aminopyrimidine to methanol is 1:2;

[0044] d. Filter out aminopyrimidine, add water and heat up to 70°C to dissolve, the ratio of aminopyrimidine to water is 1:0.5;

[0045] e. The temperature is lowered to 5-10° C., the aminopyrimidine solid is precipitated, and the pure aminopyrimidine is obtained by filtering and drying.

[0046] f, the aminopyrimidine pure product that obtains detects, as figure 1 shown.

[0047] figure 1 The information in it is shown in Table 1.

[0048] Table 1 Detection peak information

[0049]

[0050] A...

Embodiment 2

[0060] A method for purifying aminopyrimidine, the steps of which are:

[0061] a. Formylpyrimidine: sodium hydroxide: water = 1:1:3 ratio, heat up and dissolve, keep warm at 80°C for 4 hours to obtain aminopyrimidine solution;

[0062] b. Cool down to 0-5°C, the aminopyrimidine solid precipitates out, and the aminopyrimidine is filtered out;

[0063] c. Wash the aminopyrimidine solid with methanol to remove impurities, and the ratio of aminopyrimidine to methanol is 1:2;

[0064] d. Filter out aminopyrimidine, add water and heat up to 50°C to dissolve, the ratio of aminopyrimidine to water is 1:0.5;

[0065] e. The temperature is lowered to 0-5° C., the aminopyrimidine solid is precipitated, and the pure aminopyrimidine is obtained by filtering and drying.

[0066] f, the obtained pure aminopyrimidine is detected.

[0067] Aminopyrimidine content, i.e. aminopyrimidine purity, is calculated as follows:

[0068]

[0069] Wherein, A—aminopyrimidine content;

[0070] S 1...

Embodiment 3

[0077] A method for purifying aminopyrimidine, the steps of which are:

[0078] a. Formylpyrimidine: sodium hydroxide: water = 1:2:5 ratio, heat up and dissolve, keep warm at 120°C for 2 hours to obtain aminopyrimidine solution;

[0079] b. Cool down to 10-20°C, the aminopyrimidine solid precipitates out, and the aminopyrimidine is filtered out;

[0080] c. Wash the aminopyrimidine solid with methanol to remove impurities, and the ratio of aminopyrimidine to methanol is 1:2;

[0081] d. Filter out aminopyrimidine, add water and heat up to 80°C to dissolve, the ratio of aminopyrimidine to water is 1:0.5;

[0082] e. The temperature is lowered to 10-20° C., the aminopyrimidine solid is precipitated, and the pure aminopyrimidine is obtained by filtering and drying.

[0083] f, the obtained pure aminopyrimidine is detected.

[0084] Aminopyrimidine content, i.e. aminopyrimidine purity, is calculated as follows:

[0085]

[0086] Wherein, A—aminopyrimidine content;

[0087]...

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Abstract

The invention relates to the field of aminopyrimidine purification, in particular to a method for purifying aminopyrimidine. The method for purifying aminopyrimidine comprises the steps as follows: (a) subjecting a strong base solution of formylpyrimidine to a reaction to obtain an aminopyrimidine solution; (b) precipitating aminopyrimidine in the aminopyrimidine solution to obtain the aminopyrimidine; (c) washing the aminopyrimidine with methanol; and (d) dissolving the obtained aminopyrimidine by adding water and then precipitating and separating to obtain pure aminopyrimidine. By adopting the method for purifying aminopyrimidine provided by the invention, most impurities can be removed, and the purity of the obtained pure aminopyrimidine reaches 99.9% or be more than 99.9%, therefore, aguarantee is provided for sample detection and analysis.

Description

technical field [0001] The invention relates to the field of aminopyrimidine purification, in particular to a method for purifying aminopyrimidine. Background technique [0002] Vitamin B1, also known as thiamine or anti-neuritis vitamin or anti-beriberi vitamin, is a white crystal that is easily oxidized in the presence of oxidants to produce dehydrothiamine, which shows blue fluorescence when irradiated by ultraviolet light. A B vitamin composed of a pyrimidine ring and a thiazole ring combined through a methylene group. In the existing technology, the yield and quality of vitamin B1 synthesis are low. [0003] In view of this, the present invention is proposed. Contents of the invention [0004] The inventor found through a large number of experiments and analysis that 2-methyl-4-amino-5-aminomethylpyrimidine (abbreviated as aminopyrimidine) is an important intermediate product of vitamin B1 synthesis, and the content of aminopyrimidine directly affects the synthetic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/42
CPCC07D239/42
Inventor 李褦成陈英明崔胜凯严建斌
Owner 江苏兄弟维生素有限公司
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