Preparation method of L-carnitine
The technology of L-carnitine and catalyst is applied in the field of preparation of chiral substances, which can solve problems such as environmental pollution, and achieve the effects of less environmental pollution, easy availability of raw materials and low pressure.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
Embodiment 1
[0025] Example 1: Preparation of catalyst [RuCl(cymene)(S-BINAP)]Cl.
[0026] Get the chiral ligand S-BINAP (0.535g, 0.85mmol) and ruthenium compound [Ru(p-cymene)Cl 2 ] 2 (0.29g, 0.47mmol) in the three-necked bottle, under N 2 Add absolute ethanol 60mL and CH under protection 2 Cl 2 20mL, heated to 50-60°C and stirred for 20h. After removing the solvent under reduced pressure, 0.87g of reddish-brown product [RuCl(cymene)(S-BINAP)]Cl[chloro[(S)-(-)-2, 2'-bis(diphenylphosphine)-1,1'-binaphthyl](p-cymenyl)ruthenium(II) chloride].
Embodiment 2
[0027] Example 2: Preparation of intermediate (R)-(-)-4-chloro-3-hydroxybutyric acid ethyl ester.
[0028] Take 80g of ethyl 4-chloroacetoacetate in an autoclave equipped with a Teflon liner, and after the autoclave is closed, use 5kgf / cm 2 of pure H 2 (99.99%) After washing the autoclave more than 10 times, fill the autoclave with hydrogen for use. in H 2 Dissolve the catalyst [RuCl(cymene)(S-BINAP)]Cl (30 mg) in 300 mL of ethyl acetate solution under the atmosphere, carefully add it into the autoclave with a syringe, and continue to charge hydrogen to 5 kgf / cm 2 Finally, raise the temperature to about 80°C, let it stand for about 20 minutes, then start stirring, react at this temperature for 6 hours, stop the reaction, take out the material, and remove the lower alkyl ester solvent by vacuum distillation to obtain a high-purity product. The product was analyzed by GC. The conversion rate is greater than 99%, and the ee value is 96%.
Embodiment 3
[0029] Example 3: Preparation of intermediate (R)-(-)-4-bromo-3-hydroxybutyrate butyl ester.
[0030]Take 80g of 4-butyl bromoacetoacetate in an autoclave equipped with a polytetrafluoroethylene liner, and after the autoclave is closed, use 3kgf / cm 2 of pure H 2 (99.99%) After washing the autoclave more than 10 times, fill the autoclave with hydrogen for use. in H 2 Dissolve the catalyst [RuCl(cymene)(S-BINAP)]Cl (3 mg) in 300 mL of propyl acetate solution under atmosphere, carefully add it into the autoclave with a syringe, and continue to charge hydrogen to 3 kgf / cm 2 Afterwards, raise the temperature to about 120°C, let it stand for about 60 minutes, start stirring, react at this temperature for 10 hours, stop the reaction, take out the material and remove the lower alkyl ester solvent by vacuum distillation to obtain a high-purity product. The product was analyzed by GC. The conversion rate was 100%, and the ee value was 96%.
PUM
Property | Measurement | Unit |
---|---|---|
purity | aaaaa | aaaaa |
optical purity | aaaaa | aaaaa |
enantiomeric excess | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
- R&D Engineer
- R&D Manager
- IP Professional
- Industry Leading Data Capabilities
- Powerful AI technology
- Patent DNA Extraction
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