Method for preparing D-cycloserine through one-pot method
A technology of cycloserine and serine, which is applied in the field of medicine, can solve the problems of many reagents, long reaction steps, unfavorable detection of D-cycloserine residues, etc., and achieve the effects of high liquid phase purity, mild reaction, and improved atom economy
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
Embodiment 1
[0032] (1) Preparation of Intermediate I:
[0033] Add 741g of toluene to a 2000ml dry four-neck round bottom bottle, add 123.5g of 3-chloro-D-serine under stirring and install a drying tube, add 142.8g of thionyl chloride dropwise at 20-30°C; 60-70 ° C to complete the reaction of raw materials. After the reaction, excess thionyl chloride was removed in vacuum to obtain intermediate I, ie, a toluene solution of 3-chloro-D-alanyl chloride hydrochloride.
[0034] (2) Preparation of crude D-cycloserine:
[0035]Pre-prepared aqueous sodium hydroxide solution with a concentration of 35% by mass: 160g of sodium hydroxide and 300g of deionized water, and lowered the temperature to below 0°C. Take 300g of 35% sodium hydroxide aqueous solution and put it into a 2000ml four-neck round bottom flask, control the temperature at -5-5°C, add the above toluene solution and stir evenly. Then control the temperature at -5-5°C and add dropwise a solution of 83.4g of hydroxylamine hydrochlorid...
Embodiment 2
[0039] (1) Preparation of Intermediate I:
[0040] Add 741g of toluene to a 2000ml dry four-neck round bottom bottle, add 123.5g of 3-chloro-D-serine under stirring and install a drying tube, add 178.5g of thionyl chloride dropwise at 20-30°C; 50-60 ° C to complete the reaction of raw materials. After the reaction, excess thionyl chloride was removed in vacuum to obtain intermediate I, ie, a toluene solution of 3-chloro-D-alanyl chloride hydrochloride.
[0041] (2) Preparation of crude D-cycloserine:
[0042] Pre-prepared aqueous sodium hydroxide solution with a concentration of 35% by mass: 160g of sodium hydroxide and 300g of deionized water, and lowered the temperature to below 0°C. Take 300g of 35% sodium hydroxide aqueous solution and put it into a 2000ml four-neck round bottom flask, control the temperature at -5-5°C, add the above toluene solution and stir evenly. Then control the temperature at -5-5°C and add dropwise a solution of 104.3g of hydroxylamine hydrochlor...
Embodiment 3
[0046] (1) Preparation of Intermediate I:
[0047] Add 741g of toluene to a 2000ml dry four-neck round bottom bottle, add 123.5g of 3-chloro-D-serine under stirring and install a drying tube, add 178.5g of thionyl chloride dropwise at 20-30°C; 50-60 ° C to complete the reaction of raw materials. After the reaction, excess thionyl chloride was removed in vacuum to obtain intermediate I, ie, a toluene solution of 3-chloro-D-alanyl chloride hydrochloride.
[0048] (2) Preparation of crude D-cycloserine:
[0049] Pre-prepared aqueous sodium hydroxide solution with a concentration of 35% by mass: 160g of sodium hydroxide and 300g of deionized water, and lowered the temperature to below 0°C. Take 300g of 35% sodium hydroxide aqueous solution and put it into a 2000ml four-neck round bottom flask, control the temperature at -5-5°C, add the above toluene solution and stir evenly. Then control the temperature at -5-5°C and add dropwise a solution of 104.3g of hydroxylamine hydrochlor...
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