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Hydrolysis process of 2-methyl-4-amino-5-(formamidomethyl)pyrimidine

A formamidomethyl and amino technology, which is applied in the field of preparation of vitamin B1 intermediates, can solve the problems of large waste water treatment volume, difficult separation, and difficult waste water treatment, and achieves reduction of difficulty, cost saving, and high product content. Effect

Inactive Publication Date: 2018-01-19
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the product 2-methyl-4-amino-5-(aminomethyl)pyrimidine has a certain solubility in water, it is difficult to separate out, so after hydrolysis, it is directly used in the next step reaction without separation, and the by-product sodium formate of this step , the excess sodium hydroxide and water are taken to the next step as wastewater treatment, which not only affects the next reaction and separation process, but also has a large amount of wastewater treatment
With the improvement of social requirements for environmental protection, the problem of this process is becoming more and more serious. Related companies have also explored the use of 2-methyl-4-amino-5-(formylaminomethyl)pyrimidine in aqueous sodium hydroxide solution. After hydrolysis, the product 2-methyl-4-amino-5-(aminomethyl)pyrimidine generated is precipitated by cooling down, but because 2-methyl-4-amino-5-(aminomethyl)pyrimidine has certain The solubility is as high as 22.0g at room temperature, and there are many residues in the mother liquor, and the by-product sodium formate cannot be separated and purified, and the difficulty of wastewater treatment is still relatively large

Method used

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  • Hydrolysis process of 2-methyl-4-amino-5-(formamidomethyl)pyrimidine

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Effect test

Embodiment 1

[0024] The experimental flow chart is illustrated in the patent drawings figure 1 : As shown in a 2-methyl-4-amino-5-(formylmethyl) pyrimidine pilot cycle hydrolysis flow chart, comprises the steps:

[0025] (1) Add 400L of distilled water in the reflux reactor 1, add 375.75kg of 2-methyl-4-amino-5-(formamidomethyl)pyrimidine and 80.00kg of sodium hydroxide from the solid feed port, Start stirring, control the temperature at about 110°C, and react for 2 hours. After the reaction, 2000 L of toluene was added to the reaction kettle 1 to extract the main product 2-methyl-4-amino-5-(aminomethyl)pyrimidine. After half an hour, the stirring was stopped, the layers were separated, and the organic phase and the aqueous phase were released.

[0026] (2) The water phase is put into the water phase storage tank 3 through the intermediate tank 2; the toluene phase is put into the cooling kettle 9 through the intermediate tank 2, cooled to about 0°C, and the product is separated out afte...

Embodiment 2

[0031] The 400L aqueous solution that is dissolved with excess sodium hydroxide left in the water phase storage tank 8 of Example 1 is transported in the reactor 1, and replaces 400L distilled water as a solvent for mechanical application. Other process conditions and operating procedures are as in Example 1, and the raw materials are added See Table 1 for the amount and product yield.

[0032] In the above-mentioned process example: the 2-methyl-4-amino-5-(aminomethyl)pyrimidine separated twice was combined to obtain 550.01kg, and the obtained product was detected by HPLC as 2-methyl-4-amino-5 The -(aminomethyl)pyrimidine content was 99.20%.

Embodiment 3

[0034] The 400L aqueous solution that is dissolved with excess sodium hydroxide left in the aqueous phase storage tank 8 of Example 2 is transported in the reactor 1, and replaces 400L distilled water as a solvent to apply mechanically. Other process conditions and operating procedures are as in Example 1, and the raw materials are added See Table 1 for the amount and product yield

[0035] In the above-mentioned process example: the 2-methyl-4-amino-5-(aminomethyl)pyrimidine separated twice was combined to obtain 551.32kg, and the obtained product was detected by HPLC as 2-methyl-4-amino-5 The -(aminomethyl)pyrimidine content was 99.30%.

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Abstract

The invention relates to a hydrolysis process of 2-methyl-4-amino-5-(formamidomethyl)pyrimidine for preparing 2-methyl-4-amino-5-(aminomethyl)pyrimidine. The process is a hydrolysis process of 2-methyl-4-amino-5-(formamidomethyl)pyrimidine and comprises the following steps that alternative excess reaction of the two raw materials is performed, the generated product is extracted by a solvent, theproduct is obtained by cooling precipitation, and the solvent is repeatedly used with water. Compared with the prior art, in the process, the 2-methyl-4-amino-5-(formamidomethyl)pyrimidine can be fully hydrolyzed, the product content is high, and the byproduct sodium formate can be separated out. In addition, no wastewater is generated in the process, and the solvent is not consumed.

Description

technical field [0001] The present invention relates to a preparation method of a vitamin B1 intermediate, specifically a method for preparing 2-methyl-4-amino-5 by hydrolysis of 2-methyl-4-amino-5-(formylaminomethyl)pyrimidine. - the (aminomethyl)pyrimidine method. Background technique [0002] The hydrolysis of 2-methyl-4-amino-5-(formylaminomethyl)pyrimidine to 2-methyl-4-amino-5-(aminomethyl)pyrimidine is an important process in the synthesis of vitamin B1, and the reaction is as follows : [0003] [0004] The main process currently used in industrialization is the hydrolysis of 2-methyl-4-amino-5-(formylaminomethyl)pyrimidine in aqueous sodium hydroxide solution. Because the product 2-methyl-4-amino-5-(aminomethyl)pyrimidine has a certain solubility in water, it is difficult to separate out, so after hydrolysis, it is directly used in the next step reaction without separation, and the by-product sodium formate of this step , Excess sodium hydroxide and water are ...

Claims

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Application Information

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IPC IPC(8): C07D239/42C07C51/06C07C51/42C07C51/43C07C53/06
Inventor 林富荣曾天亮周永生
Owner CHANGZHOU UNIV
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