Preparation method for 3-O-alkyl ascorbic acid
A technology of an alkyl ascorbic acid and a synthesis method, which is applied in the field of preparation of 3-O-alkyl ascorbic acid, can solve the problems of complex process products, complicated post-processing, unsuitable for large-scale production and the like, and achieves environmentally friendly process, simple and feasible process , the synthesis route is simple and novel effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0016] Under the protection of nitrogen, add 10.1 g (0.1 mol) of triethylamine to 50 ml of methanol, and slowly add 20.8 g (0.1 mol) of 2-keto-L-gulonate methyl ester to the above mixture under stirring. , Add 1 gram of molecular sieve, then add 12.6 grams (0.1 mol) of dimethyl sulfate dropwise, heat to 60 degrees and react for 3 hours, distill the methanol from the reaction solution under reduced pressure, and concentrate the viscous reaction solution in ethyl acetate After flushing, it quickly passes through a silica gel column (Flash column chromatography), and stops when the 2-keto-3-O-methyl-L-gulonate methyl ester is completely flushed out. Evaporate the solvent to obtain a yellow product. Under the protection of nitrogen, dissolve the obtained yellow product in 80 ml methanol, add 9.25 g (0.11 mol) sodium bicarbonate and 1.5 g (0.02 mol) calcium fluoride, reflux for 5 hours, and distill the methanol from the reaction solution under reduced pressure The concentrated visc...
Embodiment 2
[0018] Under the protection of nitrogen, add 10.1 g (0.1 mol) of triethylamine to 50 ml of ethanol, and slowly add 22.2 g (0.1 mol) of ethyl 2-keto-L-gulonate to the above mixture under stirring. , Add 1 gram of molecular sieve, and then add 15.4 grams (0.1 mol) of diethyl sulfate dropwise, heat to 78 degrees and react for 3 hours, distill the ethanol from the reaction solution under reduced pressure, and concentrate the viscous reaction solution in ethyl acetate After flushing, it quickly passes through a silica gel column (Flash column chromatography), and stops when the 2-keto-3-O-ethyl-L-gulonate ethyl ester is completely flushed out by the dot plate. Evaporate the solvent to obtain a yellow product. Under the protection of nitrogen, dissolve the obtained yellow product in 80 ml of ethanol, add 9.25 g (0.11 mol) of sodium bicarbonate and 1.5 g (0.02 mol) of calcium fluoride, reflux for 5 hours, and distill the ethanol from the reaction solution under reduced pressure The c...
Embodiment 3
[0020] Under nitrogen protection, add 10.1 g (0.1 mol) of triethylamine to 50 ml of ethanol, and slowly add 20.8 g (0.1 mol) of 2-keto-L-gulonate methyl ester to the above mixture under stirring. , Add 1 gram of molecular sieve, then add 22.2 grams (0.1 mol) of diethyl sulfate dropwise, heat to 78 degrees for 3 hours, distill the ethanol from the reaction solution under reduced pressure, and concentrate the viscous reaction solution in ethyl acetate After flushing, it quickly passes through a silica gel column (Flash column chromatography), and stops when the 2-keto-3-O-ethyl-L-gulonate methyl ester is completely flushed out. Evaporate the solvent to obtain a yellow product. Under the protection of nitrogen, dissolve the obtained yellow product in 80 ml of ethanol, add 9.25 g (0.11 mol) of sodium bicarbonate and 1.5 g (0.02 mol) of calcium fluoride, reflux for 5 hours, and distill the ethanol from the reaction solution under reduced pressure The concentrated viscous reaction s...
PUM
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