Preparation method of alpha-formyl-beta-formamido-propionitrile alkali metal salt

A technology of formylaminopropionitrile base and aminopropionitrile, which is applied in the field of preparation of α-formyl-β-formylaminopropionitrile alkali metal salt, can solve the problems of difficult control conditions, low conversion rate and potential safety hazards And other issues

Active Publication Date: 2018-09-04
NORTHEAST PHARMA GRP
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Problems solved by technology

At present, the preparation process of α-formyl-β-formamidopropionitrile sodium salt is usually the reaction of β-aminopropionitrile with liquid sodium methoxide and CO. By controlling the reaction pressure and temperature, the product meeting the standard requirements is obtained, but this reaction Methyl formate is obtained by reacting methanol and CO in liquid sodium methoxide, and then reacts with β-aminopropionitrile. There is a large amount of methanol in the reaction system, which inhibits the forward reaction and the conversion rate is not high; the two reactions in the system are carried out simultaneously. The conditions are difficult to control, and side reactions will occur, resulting in low product quality; the use of CO in the reaction has potential safety hazards
[0003] α-formyl-β-formylaminopropionitrile alkali metal salt is soluble in water, and sodium methylate decomposes when it encounters water. Therefore, if there is water in the system, the product yield and quality will all decrease. If there is a large amount of methanol in the system, it will not It is beneficial to the positive reaction, and the quality of the alkali metal salt of α-formyl-β-formylaminopropionitrile directly affects the subsequent reaction and vitamin B 1 Therefore, a method for preparing α-formyl-β-formylaminopropionitrile alkali metal salts suitable for large-scale industrial production is developed to minimize the content of impurities and improve the production capacity of α-formyl-β-formyl The yield of amidopropionitrile alkali metal salt, and the safe and environment-friendly operating method, these are new problems to be solved urgently at present

Method used

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  • Preparation method of alpha-formyl-beta-formamido-propionitrile alkali metal salt
  • Preparation method of alpha-formyl-beta-formamido-propionitrile alkali metal salt
  • Preparation method of alpha-formyl-beta-formamido-propionitrile alkali metal salt

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Embodiment 1

[0014] Add 284g of ethyl formate into a 500mL three-necked bottle, and slowly add 35g of solid sodium ethoxide at a rate of 1.2g / min at a certain temperature (see Table 1 for the specific selection of the temperature). Add 30g of β-aminopropionitrile dropwise at a speed of min, pour the above reaction solution into a 500mL autoclave, start stirring, heat to make the temperature rise to 65-70°C, the pressure range is 5.0-6.0MPa, and it will naturally drop to 20 after 10 hours of heat preservation. ℃ discharge, suction filtration, the filter cake was washed twice with 25g ethyl formate, and the filter cake was dried at 50 ℃ to obtain 65.8g of α-formyl-β-formylaminopropionitrile yellowish solid sodium salt with a content of 90.4 %, yield 93.8%.

[0015] Table 1: The selection of solid sodium ethylate addition temperature and the amount and yield of α-formyl-β-formylaminopropionitrile sodium salt

[0016] serial number

Embodiment 2

[0018] Add 284g of ethyl formate into a 500mL three-necked flask, slowly add 43.5g of solid sodium ethylate at a rate of 1.2g / min at -10 to 0°C, raise the temperature to 10°C, and then dropwise add 30g of β-amino at a rate of 1.2g / min For propionitrile, pour the above reaction solution into a 500mL autoclave, start stirring, and heat to make the temperature rise to a certain temperature (see Table 2 for the selection of temperature). ℃ discharge, suction filtration, the filter cake was washed twice with 25g ethyl formate, and the filter cake was dried at 60 ℃ to obtain the sodium salt of α-formyl-β-formylaminopropionitrile. The yield is shown in Table 2. The mother liquor obtained after filtration was rotary-evaporated to obtain ethanol and ethyl formate, and applied mechanically to ethyl formate to react, and the residue α-formyl-β-formylaminopropionitrile sodium salt was just dissolved in a small amount of water, and then recrystallized twice with 10g of acetone. 3 g of α-fo...

Embodiment 3

[0022] Add 200g of ethyl formate into a 500mL three-necked flask, slowly add 43.5g of solid sodium ethylate at a rate of 1.5g / min at -10 to 0°C, raise the temperature to 10°C, and then dropwise add 30g of β-amino at a rate of 1.5g / min For propionitrile, pour the above reaction solution into a 500mL autoclave, start stirring, heat to make the temperature rise to 65-70°C, and the pressure range is 5.0-6.0MPa, keep warm for 10 hours and naturally drop to 30°C to discharge, rotary steaming, The mixed solvent of ethanol and ethyl formate was distilled off and applied mechanically to the reaction of preparing ethyl formate to obtain 65.2 g of α-formyl-β-formylaminopropionitrile sodium salt with a yield of 93.5%.

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Abstract

The invention belongs to a preparation method of alpha-formyl-beta-formamido-propionitrile alkali metal salt in the field of chemical synthesis. The preparation method comprises the following steps: (1) adding formic ester into a container, and slowly adding solid alkali metal C1-4 alkyl alcoholate to form a first mixture at a certain temperature, (2) controlling a temperature of the first mixture, dropwise adding beta-aminopropionitrile into the first mixture to form a second mixture, and (3) moving the second mixture into an autoclave, allowing beta-aminopropionitrile and formic ester to generate a formylation reaction to form alpha-formyl-beta-formamido-propionitrile alkali metal salt liquid, and performing filtration to form the alpha-formyl-beta-formamido-propionitrile alkali metal salt. The method is high in yield, low in cost, simple to operate and suitable for industrial massive production, and the produced alpha-formyl-beta-formamido-propionitrile alkali metal salt is high inyield and low in impurity content.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of α-formyl-β-formylaminopropionitrile alkali metal salt. Background technique [0002] α-formyl-β-formylaminopropionitrile alkali metal salt, also known as α-alkali metal formyl-β-formylaminopropionitrile, taking alkali metal sodium as an example, its molecular formula C 5 h 5 N 2 o 2 Na, is vitamin B 1 Important chemical synthesis intermediates. At present, the preparation process of α-formyl-β-formamidopropionitrile sodium salt is usually the reaction of β-aminopropionitrile with liquid sodium methoxide and CO. By controlling the reaction pressure and temperature, the product meeting the standard requirements is obtained, but this reaction Methyl formate is obtained by reacting methanol and CO in liquid sodium methoxide, and then reacts with β-aminopropionitrile. There is a large amount of methanol in the reaction system, which inhibits the forward r...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/30
CPCC07C253/30C07C255/30
Inventor 杨会芬张莉曲壮志
Owner NORTHEAST PHARMA GRP
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