Piperonal preparation method
A technology of piperonal and glyoxylic acid, applied in the field of medicine and chemical industry, can solve the problems of deep yarn-dyed weaving, low decarboxylation efficiency, easy to produce carbonization, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
Embodiment 1
[0013] In a three-neck flask, add 1.5g of water, 10g of glyoxylic acid (40%), and 10g of sulfuric acid under stirring, cool down to 0-5°C, slowly add 6g of piperonylcycline dropwise, keep the reaction for 5 hours, and add 80mL of water to dilute , and suction filtered to obtain 3,4-dimethoxymandelic acid and dilute sulfuric acid mother liquor;
[0014] In a three-neck flask, add 70% dilute sulfuric acid mother liquor, 3,4-dimethoxymandelic acid and 80ml of methylene chloride, add 18mL of 3% dilute nitric acid dropwise at 20°C, after the addition is complete, heat up to 40°C, After reacting for 3 hours, the temperature was lowered to separate the layers, the water layer was separated, the oil layer was washed with water until neutral, and the solvent was evaporated to constant weight under reduced pressure to obtain 6 g of piperonal, with a yield of 81%.
Embodiment 2
[0016] In a three-necked flask, add 1.6g of water, 10.5g of glyoxylic acid, and 10.5g of sulfuric acid under stirring, cool down to 0-5°C, slowly add 6g of piperonylcycline dropwise, and keep it warm for 7 hours, add 90mL of water to dilute, and pump Filter to obtain 3,4-dimethoxymandelic acid and dilute sulfuric acid mother liquor;
[0017] In a three-neck flask, add 50% dilute sulfuric acid mother liquor, 3,4-dimethoxymandelic acid and 80 mL of dichloromethane, add 19 mL of 3% dilute nitric acid dropwise at 20°C, after the addition is complete, heat up to 40°C, After reacting for 3 hours, the temperature was lowered to separate the layers, the water layer was separated, the oil layer was washed with water until neutral, and the solvent was evaporated to constant weight under reduced pressure to obtain 6.2 g of piperonal, with a yield of 84%.
Embodiment 3
[0019] In a three-necked flask, add 1.7g of water, 11g of glyoxylic acid, and 11g of sulfuric acid under stirring, cool down to 0-5°C, slowly add 6g of piperonylcycline dropwise, and keep it warm for 8 hours, dilute with 100mL of water, and filter with suction. Obtain 3,4-dimethoxymandelic acid and dilute sulfuric acid mother liquor;
[0020] In a three-necked flask, add 30% dilute sulfuric acid mother liquor, 3,4-dimethoxymandelic acid and 80 mL of dichloromethane, add 20 mL of 3% dilute nitric acid dropwise at 20°C, after the addition is complete, heat up to 40°C, React for 3 hours, lower the temperature, separate the layers, remove the water layer, wash the oil layer with water until neutral, and evaporate the solvent to constant weight under reduced pressure to obtain 6.4 g of piperonal, with a yield of 87%.
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