Method for synthesizing citric acid diphenhydramine
A diphenhydramine citrate and synthesis method technology, applied in chemical instruments and methods, carboxylate preparation, organic compound preparation, etc., can solve the problems of cumbersome and complicated operations, low product yields, etc., and achieve simplified operations steps, simplify the purification steps, and shorten the production cycle
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Example Embodiment
[0021] Embodiment 1, the synthesis of benzyl alcohol-β-chloroethyl ether
[0022] 92 g of benzyl alcohol, 40 g of chloroethanol, and 21.8 ml of sulfuric acid with a mass fraction of 98% were added to the three-necked flask (the molar ratio of benzyl alcohol, chloroethanol and sulfuric acid was 1:1:0.8), and the temperature was raised to 70 °C for the insulation reaction. The reaction progress was monitored by thin-layer chromatography, the reaction was completed in 6 hours, the layers were allowed to stand, the upper layer of oily liquid was collected, washed three times with a sodium carbonate solution with a mass fraction of 25%, and then washed three times with hot water at a temperature of 60 °C, That is, bisbenzyl alcohol-β-chloroethyl ether was prepared with a yield of 78.5%.
[0023]
Example Embodiment
[0024] Embodiment 2, the synthesis of benzyl alcohol-β-chloroethyl ether
[0025] 92 g of benzyl alcohol, 52.3 g of chloroethanol, and 16.3 ml of sulfuric acid with a mass fraction of 98% were added to the three-necked flask (the molar ratio of benzyl alcohol, chloroethanol and sulfuric acid was 1:1.3:0.6), and the temperature was raised to 100 °C for insulation reaction. , monitor the reaction progress by thin layer chromatography, the reaction is completed in 4 hours, stand for stratification, collect the upper oily liquid, wash 3 times with sodium carbonate solution with a mass fraction of 15%, and then wash 3 times with hot water at a temperature of 80 ° C , namely the preparation of bis-benzyl alcohol-β-chloroethyl ether with a yield of 84.3%.
[0026]
Example Embodiment
[0027] Embodiment 3, the synthesis of benzyl alcohol-β-chloroethyl ether
[0028] Add 92 g of benzyl alcohol, 60.4 g of chloroethanol, and 10.9 ml of sulfuric acid with a mass fraction of 98% into a three-necked flask (the molar ratio of benzyl alcohol, chloroethanol and sulfuric acid is 1:1.5:0.4), and the temperature is raised to 130 ° C for insulation reaction , use thin layer chromatography to monitor the reaction process, the reaction is completed in 3 hours, stand for stratification, collect the upper oily liquid, wash 3 times with sodium carbonate solution with a mass fraction of 5%, and then wash 3 times with hot water at a temperature of 100 ° C , that is, to obtain bisbenzyl alcohol-β-chloroethyl ether with a yield of 73.6%.
[0029]
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.
© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap