Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of preparation method of racemic ketone calcium isoleucine

A technology of racemic ketone isoleucine calcium and sodium isopropoxide, which is applied in the field of drug synthesis, can solve the problems of high cost, large negative impact on the environment, and many reaction raw materials, and achieves simple operation, mild conditions, and low toxicity. Effect

Active Publication Date: 2016-04-06
SHAOXING MINSHENG PHARMA
View PDF3 Cites 1 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of racemic ketone calcium isoleucine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] At 25°C, drop 300kg of diethyl oxalate into 390kg of 28% sodium methoxide methanol solution, keep stirring for half an hour after dropping, add 200kg of 2-methylbutyraldehyde, keep warm for half an hour after adding, at a temperature not greater than 25°C Under certain conditions, add 30% sodium hydroxide aqueous solution, keep it warm for 5 hours after dripping, add 70kg of hydrochloric acid dropwise, stir for half an hour, add 600kg of methyl isobutyl ketone for extraction three times, add 100kg of purified water to the organic phase, and add 30% sodium hydroxide Aqueous solution to adjust the pH value to 5.8, layering, adding 30% sodium hydroxide aqueous solution to the organic phase to adjust the pH value to 5.8, layering, merging the aqueous phase, merging the aqueous phase, adding 30% sodium hydroxide aqueous solution to adjust the pH value to 8.8, Add 300kg of calcium chloride aqueous solution at no lower than 20°C, keep warm and stir for 2 hours after dripping, s...

Embodiment 2

[0033] At 25°C, drop 233.6 kg of dimethyl oxalate into 389 kg of 28% sodium ethoxide ethanol solution, keep stirring for half an hour after dropping, add 159 kg of 2-methylbutyraldehyde, keep warm for half an hour after adding, at a temperature not greater than 25°C Under certain conditions, add 30% sodium hydroxide aqueous solution, keep warm for 5 hours after dropping, add 58kg of hydrochloric acid dropwise, stir for half an hour, add 600kg of methyl isobutyl ketone for extraction three times, add 100kg of purified water to the organic phase, and add 30% sodium hydroxide Aqueous solution to adjust the pH value to 5.8, layering, adding 30% sodium hydroxide aqueous solution to the organic phase to adjust the pH value to 5.8, layering, merging the aqueous phase, adding 30% sodium hydroxide aqueous solution to adjust the pH value to 8.8, at least Add 232kg of calcium chloride aqueous solution at 20°C, keep stirring for 2 hours after dripping, slowly cool down to 5°C, keep warm fo...

Embodiment 3

[0035] Example 3: The difference between this example and Example 1 is that ammonia water is used instead of 30% sodium hydroxide aqueous solution to adjust the pH value, and 190 kg of refined dry product is obtained with a total yield of 81.7%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for preparing calcium 3-methyl-2-oxovalerate. The method comprises the following steps of: dripping diethyl oxalate into an alcoholic solution of sodium alkoxide; dripping 2-methyl butyraldehyde, keeping the temperature, stirring, adding an alkali solution, regulating the acid after heat insulation is ended, extracting, and adding a certain amount of water into an extracting solution; adding the alkali solution to regulate the pH, dripping an aqueous solution of calcium chloride for salifying to obtain the coarse 3-methyl-2-oxovalerate product; and refining the coarse 3-methyl-2-oxovalerate product in a mixed solvent of purified water and organic solvent, and obtaining the refined 3-methyl-2-oxovalerate product. The process is mild in reaction conditions, easy to operate, fewer in steps, high in yield and high in quality, the adopted raw materials are cheap and basically do not cause pollution, waste gas and lots of waste residues are avoided, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a chemical synthesis preparation method for racemic ketoisoleucine calcium. Calcium racemic ketoisoleucine is one of the main components of compound α-ketoacid tablets (Kaitong). 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 ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/185C07C51/41
Inventor 邢亚军黄希傅小明
Owner SHAOXING MINSHENG PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com