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Preparation of calcium 3-methyl-2-oxovalerate with one-step method

A technology of calcium racemic ketone isoleucine and one-step method is applied in the field of preparing calcium racemic ketone isoleucine by one-step method, and can solve the problems of ineffective utilization of raw materials, unfavorable atom economy, large negative impact on the environment, and the like, Achieving the effect of highly competitive market advantage, convenient large-scale production and low cost

Active Publication Date: 2019-12-31
福安药业集团重庆博圣制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this route is that there are many reaction raw materials, which is not conducive to atom economy, can not effectively use raw materials, high cost, and has a relatively large negative impact on the environment.

Method used

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  • Preparation of calcium 3-methyl-2-oxovalerate with one-step method
  • Preparation of calcium 3-methyl-2-oxovalerate with one-step method
  • Preparation of calcium 3-methyl-2-oxovalerate with one-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Preparation of wet product of racemic ketoisoleucine calcium crude product

[0034] Add 100g hydantoin, 90g butanone, 85g monoethanolamine, and 300g water into the reaction tank, raise the temperature to 72°C, and react for 7.5 hours. After the reaction, cool down to 30-40°C, add 165g of sodium hydroxide, and continue to heat up to 83°C , the reaction time is 7.5 hours, lower the temperature to 30-40°C, add hydrochloric acid to adjust the pH value to 3-4, then add 120g calcium chloride, lower the temperature to 20-30°C, grow crystals for 2-3 hours, and centrifuge to obtain racemic ketone Calcium isoleucine crude product wet product, wet weight 182g.

[0035] 2. Preparation of racemic ketoisoleucine calcium

[0036] Add 182g wet product of racemic ketoisoleucine calcium crude product into the reaction tank, add 500g ethanol, heat up to 60-70°C to dissolve, add 5g activated carbon to decolorize after dissolving, filter, and slowly cool the filtrate to 25-35°C for heat...

Embodiment 2

[0038] 1. Preparation of wet product of racemic ketoisoleucine calcium crude product

[0039] Add 100g hydantoin, 80g butanone, 80g monoethanolamine, and 300g water into the reaction tank, raise the temperature to 68°C, and react for 7.0 hours. After the reaction, cool down to 30-40°C, add 150g sodium hydroxide, and continue to heat up to 80°C , the reaction time is 7.0 hours, lower the temperature to 30-40°C, add hydrochloric acid to adjust the pH value to 3-4, then add 115g calcium chloride, lower the temperature to 20-30°C, grow crystals for 2-3 hours, and centrifuge to obtain racemic ketone Calcium isoleucine crude product wet product, wet weight 173g.

[0040] 2. Preparation of racemic ketoisoleucine calcium

[0041] Add 173g wet product of racemic ketoisoleucine calcium crude product into the reaction tank, add 500g ethanol, heat up to 60-70°C to dissolve, add 5g activated carbon to decolorize after dissolving, filter, and slowly cool the filtrate to 25-35°C for heat pr...

Embodiment 3

[0043] 1. Preparation of wet product of racemic ketoisoleucine calcium crude product

[0044] Add 100g hydantoin, 90g butanone, 80g monoethanolamine, and 300g water into the reaction tank, raise the temperature to 75°C, and react for 8.0 hours. After the reaction, cool down to 30-40°C, add 160g of sodium hydroxide, and continue to heat up to 80°C , the reaction time is 7.0 hours, lower the temperature to 30-40°C, add hydrochloric acid to adjust the pH value to 3-4, then add 120g calcium chloride, lower the temperature to 20-30°C, grow crystals for 2-3 hours, and centrifuge to obtain racemic ketone Calcium isoleucine crude product wet product, wet weight 177g.

[0045] 2. Preparation of racemic ketoisoleucine calcium

[0046] Add 177g wet product of racemic ketoisoleucine calcium crude product into the reaction tank, add 500g ethanol, heat up to 60-70°C to dissolve, add 5g activated carbon to decolorize after dissolving, filter, and slowly cool the filtrate to 25-35°C for heat...

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Abstract

The invention belongs to the technical field of pharmacy, and particularly relates to a method for preparing 3-methyl-2-oxovalerate through a one-step method. According to the one-step method, hydantoin and butanone are used as raw materials and are reacted in the presence of a solvent and monoethanolamine; after reaction, sodium hydroxide is added for hydrolysis, salification and crystallizationare carried out to obtain a crude wet product of 3-methyl-2-oxovalerate, and then dissolution, filtration, crystallization and drying are performed to obtain3-methyl-2-oxovalerate. The obtained product has the advantages of high purity, high yield, low cost, no need of refining the product subsequently, less process equipment and convenience for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a method for preparing racemic ketoisoleucine calcium in one step. Background technique [0002] Calcium racemic ketoisoleucine is one of the main components of compound α-ketoacid tablets (Kaitong). α-ketoacids and their derivatives have shown increasingly broad application prospects in food, daily chemicals and medicine. In food applications, it can be used as a component of sports nutrition drinks; in functional skin care cosmetics, it can play a very good role in moisturizing, anti-wrinkle, anti-shrinkage, anti-aging and anti-allergy. In medical applications, compound α-ketoacid tablets can treat damage caused by chronic renal insufficiency, and can be used as a specific drug for treating uremia. For patients with renal failure, taking compound α-ketoacid tablets, combined with a low-protein diet, can reduce hyperfiltration of glomeruli and protect nephrons. Fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/185C07C51/41
CPCC07C51/00C07C51/412C07C59/84
Inventor 袁明华章永强洪荣川丁东张雄车瑶罗浩
Owner 福安药业集团重庆博圣制药有限公司
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