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One-step preparation of racemic ketoisoleucine calcium

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 advantages, convenient large-scale production and low cost

Active Publication Date: 2022-05-27
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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  • One-step preparation of racemic ketoisoleucine calcium
  • One-step preparation of racemic ketoisoleucine calcium
  • One-step preparation of racemic ketoisoleucine calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Preparation of the wet product of the crude calcium isoleucine racemate

[0034] Add 100g hydantoin, 90g butanone, 85g monoethanolamine, 300g water to the reaction tank, heat up to 72°C, react for 7.5 hours, cool down to 30~40°C after the reaction, add 165g sodium hydroxide, continue to heat up to 83°C , the reaction time is 7.5 hours, cool down to 30~40 ℃, add hydrochloric acid to adjust pH value to 3~4, then add 120g calcium chloride, cool down 20~30 ℃, grow crystal for 2~3 hours, centrifuge to obtain racemic ketone Crude calcium isoleucine wet product, wet weight 182g.

[0035] 2. Preparation of Calcium Racemone Isoleucine

[0036] In the reaction tank, add 182g of crude wet product of racemic isoleucine calcium, add 500g of ethanol, heat up to 60~70℃ to dissolve, add 5g of activated carbon to decolorize after dissolving, filter, and slowly cool the filtrate to 25~35℃ for thermal insulation analysis Crystallize for 2-3 hours, filter, and wash the filter cake wit...

Embodiment 2

[0038] 1. Preparation of the wet product of the crude calcium isoleucine racemate

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

[0040] 2. Preparation of Calcium Racemone Isoleucine

[0041] In the reaction tank, add 173 g of the wet product of the crude calcium isoleucine racemate, add 500 g of ethanol, heat up to 60-70 °C to dissolve, add 5 g of activated carbon to decolorize after the solution is clear, filter, and slowly cool the filtrate to 25-35 °C for thermal insulation analysis. Crystallize for 2-3 hours, filter, ...

Embodiment 3

[0043] 1. Preparation of the wet product of the crude calcium isoleucine racemate

[0044] Add 100g hydantoin, 90g butanone, 80g monoethanolamine, 300g water to the reaction tank, heat up to 75°C, react for 8.0 hours, cool down to 30~40°C after the reaction, add 160g sodium hydroxide, continue to heat up to 80°C , the reaction time is 7.0 hours, cool down to 30~40 ℃, add hydrochloric acid to adjust pH value to 3~4, then add 120g calcium chloride, cool down 20~30 ℃, grow crystal for 2~3 hours, centrifuge to obtain racemic ketone Crude calcium isoleucine wet product, wet weight 177g.

[0045] 2. Preparation of Calcium Racemone Isoleucine

[0046] In the reaction tank, add 177g of the crude wet product of racemic ketone isoleucine calcium, add 500g of ethanol, heat up to 60-70°C to dissolve, add 5g of activated carbon to decolorize after the solution is clear, filter, and the filtrate is slowly cooled to 25-35°C for thermal insulation analysis. Crystallize for 2-3 hours, filter...

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Abstract

The invention belongs to the technical field of pharmacy, and in particular relates to a method for preparing racemic ketoisoleucine calcium in one step. The one-step method uses hydantoin and methyl ethyl ketone as raw materials, reacts in the presence of a solvent and monoethanolamine, adds sodium hydroxide after the reaction for hydrolysis, salt formation, and crystallization to obtain a wet crude product of racemic ketone isoleucine calcium, and then undergoes Dissolving, filtering, crystallizing and drying to obtain racemic ketoisoleucine calcium. The obtained product has high purity, high yield, low cost, no subsequent refining of the product, less process equipment, and is convenient 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 calcium racemic ketone isoleucine by one-step method. Background technique [0002] Calcium racemone isoleucine is one of the main components of compound α-ketoacid tablets (Kaitong). Alpha-keto acids and their derivatives show 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 good role in moisturizing, anti-wrinkle, anti-shrinkage, anti-aging and anti-allergic. In medical application, compound α-ketoacid tablets can treat damage caused by chronic renal insufficiency, and can be used as a special drug for the treatment of uremia. Taking compound α-ketoacid tablets in combination with a low-protein diet in patients with renal failure can reduce glomerular hyperfiltration and protect neph...

Claims

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Application Information

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Patent Type & Authority Patents(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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