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Biotin and preparation method thereof

A biotin and product technology, applied in the direction of organic chemistry and the like, can solve the problems of insufficient environmental protection, economy, difficulty in recovering benzyl bromide, etc., and achieve the effects of good commercial value, less burning residue and low heavy metal content

Pending Publication Date: 2022-07-26
浙江花园营养科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the whole process of this method will produce a large amount of waste water, and the generated benzyl bromide will be extracted with an organic solvent, which will cause difficulty in the recovery of benzyl bromide, which is not environmentally friendly and economical enough.

Method used

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  • Biotin and preparation method thereof
  • Biotin and preparation method thereof

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Experimental program
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Embodiment 1

[0032] A preparation method of biotin, comprising the following steps:

[0033] (1) Preparation of product 1 and product 2: 100g of fumaric acid and 500mL of deionized water were added to the reaction kettle, heated to 120°C, slowly added dropwise with 100g of bromine, reacted at 120°C for 3 hours, and cooled to At room temperature, the solid product was obtained by filtration and drying; then 100 g of the solid product, 150 g of benzylamine, and 500 mL of toluene were added to the reaction kettle, and the reaction was carried out at 120 ° C for 6 h. White solid; 100g white solid, 1000g 30% liquid caustic soda are then added to the reactor to dissolve, and 500g massfraction is added dropwise simultaneously to be 30% two (trichloromethyl) carbonate toluene solution, in the dropping process, the dropwise temperature is controlled less than 80°C, after the dropwise addition was completed, the mixture was left to stand for stratification, the organic layer was distilled under redu...

Embodiment 2

[0043] A preparation method of biotin, comprising the following steps:

[0044] (1) Preparation of product 1 and product 2: 100g of fumaric acid and 500mL of deionized water were added to the reaction kettle, heated to 120°C, slowly added dropwise with 200g of bromine, reacted at 125°C for 2h, cooled to At room temperature, the solid product was obtained by filtration and drying; then, 100 g of the solid product, 200 g of benzylamine, and 500 mL of toluene were added to the reaction kettle, and the reaction was carried out at 125 ° C for 5 h. White solid; 100g white solid, 1200g 30% liquid caustic soda are added into the reactor to dissolve subsequently, and 800g massfraction is added dropwise simultaneously to be 35% bis(trichloromethyl) carbonate toluene solution, and the dropping temperature is controlled less than 80°C, after the dropwise addition was completed, the layers were left to stand, the organic layer was distilled under reduced pressure, filtered and dried to obt...

Embodiment 3

[0054] A preparation method of biotin, comprising the following steps:

[0055] (1) Preparation of product 1 and product 2: 100g of fumaric acid and 500mL of deionized water were added to the reactor, heated to 120°C, slowly added dropwise with 300g of bromine, reacted at 130°C for 1 h, cooled to At room temperature, the solid product was obtained by filtration and drying; then 100 g of the solid product, 250 g of benzylamine, and 500 mL of toluene were added to the reaction kettle, and the reaction was carried out at 130 ° C for 4 hours. White solid; 100g white solid, 1500g 30% liquid caustic soda are added into the reactor to dissolve subsequently, and 1000g massfraction is added dropwise simultaneously to be 40% bis(trichloromethyl) carbonate toluene solution, and the dropping temperature is controlled less than 80°C, after the dropwise addition was completed, the layers were left to stand, the organic layer was distilled under reduced pressure, filtered and dried to obtain...

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PUM

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Abstract

The invention discloses biotin and a preparation method thereof. The preparation method comprises the following steps: (1) preparing a product 1 and a product 2; (2) preparing a product 3; (3) preparation of thiolactone; (4) preparing an ethanol solution of the Grignard substance; (5) preparing a hydrogenated product ethanol solution; (6) synthesizing biotin; and (7) refining biotin. The invention provides the biotin and the preparation method thereof, the method is safe and environment-friendly, the d-biotin can be simply and conveniently obtained with high yield, the industrial production efficiency of the d-biotin is improved, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a biotin and a preparation method thereof. Background technique [0002] Biotin also known as vitamin B 7 , which mainly exists in animals and plants in nature, is an indispensable vitamin for maintaining the normal movement of the human body, and is also a necessary substance for the synthesis of vitamin C. It is a bicyclic compound containing 3 asymmetric carbon atoms, and there are 8 isomers in total, but only the all-cis structure of d-biotin has physiological activity. d-Biotin is a water-soluble B vitamin, also known as vitamin H and coenzyme R. Biotin is commonly found in animals and plants in nature, especially in the liver, kidney, spleen, yeast and egg yolk of animals. Biotin is a coenzyme of carboxylase and an important coenzyme in the intermediate metabolism of sugar, protein and fat. If the human body lacks biotin, it will cause nutritional ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D495/04
CPCC07D495/04
Inventor 张洪真刘建刚郭阳刘小平
Owner 浙江花园营养科技有限公司
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