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Preparation method and application of alpha-sodio formyl-beta-formylaminopropionitrile

A technology of formylaminopropionitrile and sodium formyl, which is applied in the field of preparation of α-sodium formyl-β-formylaminopropionitrile, can solve the problem of low synthesis yield of sodium and high unit consumption of methyl formate , large molar number of methyl formate, etc., to reduce the generation of high boiling substances, increase the synthesis yield, and reduce the consumption

Active Publication Date: 2021-05-11
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Existing synthetic technique is because the synthetic yield of sodium generation is relatively low because of problems such as the reaction balance of sodium generation, and the synthetic yield of sodium generation is only about 64~65%, and the molar number of methyl formate is larger in the reaction process of sodium generation, and solid Sodium methoxide produces certain side reactions leading to higher unit consumption of methyl formate

Method used

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preparation example Construction

[0031] According to one aspect of the present invention, a kind of preparation method of α-sodioformyl-β-formamidopropionitrile, described preparation method comprises the following steps:

[0032] (a), β-aminopropionitrile and methyl formate are mixed for formylation reaction to obtain pre-acylation liquid;

[0033] (b), adding sodium methoxide and isopropanol to the preacylation solution and mixing successively, and then performing a synthesis reaction to obtain a solution containing α-sodium formyl-β-formamidopropionitrile;

[0034] (c), the solution containing α-sodioformyl-β-formamidopropionitrile prepared in step (b) is successively filtered and dried to obtain α-sodioformyl-β-formamidopropionitrile .

[0035] The preparation method of α-sodium formyl-β-formamidopropionitrile provided by the application, the preparation method first mixes β-aminopropionitrile and methyl formate to carry out formylation reaction to obtain a preacylation liquid; then Sodium methoxide and...

Embodiment 1

[0062] A preparation method of α-sodioformyl-β-formamidopropionitrile, said preparation method comprising the following steps:

[0063] 1, add 100g beta-aminopropionitrile, 235g methyl formate (content 93%) in there-necked flask, control 50 ℃ of reaction 3 hours, reaction generates the preacylation liquid that contains beta-formamidopropionitrile and methyl alcohol; Then The temperature of the pre-acylation solution after the heat preservation was completed was lowered to 0° C., and then 104 g of sodium methoxide (content 96%) was added to the pre-acylation liquid for mixing, and the temperature of the mixed solution was kept at 8° C. during the addition and mixing of the sodium methoxide.

[0064] 2. Pour all the reaction solution and 140g of isopropanol in the three-neck flask into the autoclave, close the lid of the autoclave, heat up to 80°C for 5 hours under agitation, and react for 5 hours. After the heat preservation is completed, cool down to 10°C and filter Dry to obt...

Embodiment 2

[0067] A preparation method of α-sodioformyl-β-formamidopropionitrile, said preparation method comprising the following steps:

[0068] 1, add 100g beta-aminopropionitrile, 235g methyl formate (content 93%) in the there-necked flask, control 20 ℃ of reaction 1 hour, reaction generates the preacylation liquid that contains beta-formamidopropionitrile and methyl alcohol; Then The temperature of the pre-acylation solution after the heat preservation was completed was lowered to 0° C., and then 104 g of sodium methoxide (content 96%) was added to the pre-acylation liquid for mixing, and the temperature of the mixed solution was kept at 8° C. during the addition and mixing of the sodium methoxide.

[0069] 2. Pour all the reaction solution and 140g of isopropanol in the three-neck flask into the autoclave, close the lid of the autoclave, heat up to 70°C for 4 hours while stirring, and cool down to 20°C after the heat preservation is over, filter Dry to obtain solid α-sodium formyl-...

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Abstract

The invention provides a preparation method and application of alpha-sodio formyl-beta-formylaminopropionitrile, and relates to the technical field of chemical synthesis. The preparation method of the alpha-sodio formyl-beta-formylaminopropionitrile comprises the following steps of: firstly, mixing beta-aminopropionitrile with methyl formate, and carrying out formylation reaction to obtain a pre-acylation solution; then sequentially adding sodium methoxide and isopropanol into the pre-acylation solution to be mixed, and conducting a synthetic reaction to obtain a solution containing alpha-sodium formyl-beta-formylaminopropionitrile; and finally, sequentially filtering and drying to obtain the alpha-sodio formyl-beta-formylaminopropionitrile. According to the preparation method, the sodio synthesis yield is effectively improved, and detection shows that the sodio synthesis yield can reach about 90% and is far higher than the existing sodio synthesis yield which is about 64%; and meanwhile, the preparation method also has the effects of reducing the consumption of methyl formate and reducing the generation of sodio mother liquor high-boiling residues.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of α-sodioformyl-β-formamidopropionitrile and its application. Background technique [0002] α-sodium formyl-β-formylaminopropionitrile, referred to as sodium formyl, is a key intermediate in the synthesis of vitamin B1, which is directly related to the production cost and quality of vitamin B1. Existing synthesis technique is because the synthetic yield of sodium generation is relatively low because of problems such as the reaction balance of sodium generation, and the synthetic yield of sodium generation is only about 64~65%, and the molar number of methyl formate is larger in the reaction process of sodium generation, and solid Sodium methoxide produces certain side reactions leading to higher unit consumption of methyl formate. [0003] Therefore, a novel α-sodium formyl-β-formamidopropionitrile synthesis process has been developed to improve ...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/29C07D415/00
CPCC07C253/30C07D415/00C07C255/29
Inventor 王诚李褦成陈英明严建斌
Owner 江苏兄弟维生素有限公司
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