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Green synthesis method of vitamin B1 intermediate

A synthesis method and compound technology, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve problems such as difficulty in controlling the amount of chlorinated reagents, troublesome post-processing, environmental hazards, etc., and achieve industrialization. The effect of application, less corrosiveness of equipment and low production cost

Pending Publication Date: 2021-12-24
ZHEJIANG NHU CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method will produce a large amount of toxic and harmful exhaust gases such as sulfur dioxide and hydrochloric acid, which are very harmful to the human body and the environment, and the post-treatment is more troublesome. , easy to produce by-products such as polychlorination

Method used

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  • Green synthesis method of vitamin B1 intermediate
  • Green synthesis method of vitamin B1 intermediate
  • Green synthesis method of vitamin B1 intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Take 220g H 2 O, 40g α-acetyl-γ-butyrolactone (0.3122mol), 0.618g cuprous chloride, 0.786g manganese chloride, add in a 500mL tetrafluoroethylene-lined airtight autoclave with stirring and cooling reflux device , oxygen replacement 3 times, and then feed oxygen into the autoclave until the pressure in the autoclave is about 1.36MPa, and keep the pressure in the autoclave at about 1.36MPa, raise the temperature in the autoclave to 85°C, and react for 10h under stirring. After the reaction, the temperature in the kettle was slowly lowered to 25°C, and the oxygen in the kettle was evacuated, and then HCl was introduced until the initial reaction pressure in the kettle was 0.48MPa, then the introduction was stopped, and the reaction was continued for 2 hours under stirring. Then slowly heat up to 70°C, continue to react for 2h under stirring, after the reaction is over, cool to room temperature, connect the exhaust port of the autoclave to the tail gas absorption device and...

Embodiment 2

[0055] Take 220g H 2 O, 40g α-acetyl-γ-butyrolactone (0.3122mol), 0.618g cuprous chloride, 1.105g cobalt acetate, join in the 500mL tetrafluoroethylene-lined airtight autoclave with stirring and cooling reflux device, Oxygen was replaced 3 times, and then oxygen was introduced into the autoclave until the pressure inside the autoclave was about 1.36 MPa, and the pressure inside the autoclave was maintained at about 1.36 MPa. After the reaction, the temperature in the kettle was slowly lowered to 25°C, and the oxygen in the kettle was evacuated, and then HCl was introduced until the initial reaction pressure in the kettle was 0.32 MPa, then the introduction was stopped, and the reaction was continued for 2 hours under stirring. Then slowly heat up to 70°C, continue to react for 2h under stirring, after the reaction is over, cool to room temperature, connect the exhaust port of the autoclave to the tail gas absorption device and open it, take a sample after emptying, and use the...

Embodiment 3

[0057] Take 300g H 2 O, 40g α-acetyl-γ-butyrolactone (0.3122mol), 0.618g cuprous chloride, 1.295g ruthenium trichloride, add to a 500mL closed autoclave lined with tetrafluoroethylene with stirring and cooling reflux device In the autoclave, oxygen was replaced three times, and then oxygen was introduced into the autoclave until the pressure in the autoclave was 0.85MPa, and the pressure in the autoclave was maintained at about 0.85MPa. After the reaction, the temperature in the kettle was slowly lowered to 25°C, and the oxygen in the kettle was evacuated, and then HCl was introduced until the initial reaction pressure in the kettle was 0.32 MPa, then the introduction was stopped, and the reaction was continued for 2 hours under stirring. Then slowly heat up to 70°C, continue to react for 2h under stirring, after the reaction is over, cool to room temperature, connect the exhaust port of the autoclave to the tail gas absorption device and open it, take a sample after emptying,...

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Abstract

The invention discloses a green synthesis method of a vitamin B1 intermediate, which comprises the following steps of reacting alpha-acetyl-gamma-butyrolactone in a solvent under an aerobic condition in the presence of a catalyst to generate alpha-hydroxy acetyl-gamma-butyrolactone, then introducing hydrogen chloride into a reaction system, and sequentially carrying out substitution reaction and hydrolysis decarboxylation reaction to generate a vitamin B1 intermediate, namely 3-chloro-5-hydroxy-2-pentanone. The catalyst comprises copper salt Lewis acid. The method for synthesizing the 3-chloro-5-hydroxy-2-pentanone is more environment-friendly, small in equipment corrosion and higher in yield, can be carried out by a one-pot method, is simpler to operate, is lower in production cost, and is more suitable for industrial application.

Description

technical field [0001] The invention relates to the technical field of vitamin B1 production, in particular to a green synthesis method of vitamin B1 intermediate 3-chloro-5-hydroxyl-2-pentanone. Background technique [0002] Vitamin B1, also known as thiamine, as the first discovered water-soluble vitamin and the vitamin with the longest synthetic route, has attracted widespread attention. It is used to solve neuritis, myocarditis, indigestion and other diseases. Disease prevention and treatment. Its key intermediate thiothiamine (C) is industrially prepared from diaminopyrimidine (A) and 3-chloro-5-hydroxyl-2-pentanone (B) as starting materials through a series of reactions, as follows The formula shows: [0003] [0004] 3-Chloro-5-hydroxy-2-pentanone is an important intermediate for the synthesis of thiothiamine. Regarding the synthesis of 3-chloro-5-hydroxy-2-pentanone, the existing technology mainly uses α-acetyl-γ - Butyrolactone as the starting material, under ...

Claims

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Application Information

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IPC IPC(8): C07C45/61C07C49/173
CPCC07D307/33C07C45/61C07C49/173Y02P20/584
Inventor 于洋张庭兰王钰王玉岗俞宏伟王俊美杨辉
Owner ZHEJIANG NHU CO LTD
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