A kind of preparation method of 1-(4-methoxy-benzyl)-2-methyl-octahydroisoquinoline
A technology of octahydroisoquinoline and methyl isoquinoline, applied in the direction of organic chemistry and the like, can solve the problems of complex synthesis, low yield, difficulty in obtaining raw materials, etc., and achieves safe reaction conditions, high yield, and reduced production costs. Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
preparation example Construction
[0020] The present invention provides a kind of preparation method of 1-(4-methoxy-benzyl)-2-methyl-1,2,3,4,5,6,7,8-octahydroisoquinoline, first 1,2,3,4,5,6,7,8-octahydro-1-(methoxyphenyl)methylisoquinoline is dissolved in a solvent, then add formaldehyde solution, after stirring, then add catalyst, and Introduce hydrogen to carry out catalytic hydrogenation reaction. After the reaction is over, filter out the catalyst and separate by precipitation and distillation to obtain 1-(4-methoxy-benzyl)-2-methyl-1,2,3, 4,5,6,7,8-Octahydroisoquinoline.
[0021] specifically:
[0022] The solvent is methanol, ethanol or isopropanol.
[0023] The formaldehyde solution contains 30%wt formaldehyde.
[0024] The catalyst is Raeburg nickel or palladium carbon.
[0025] The mass ratio of the 1,2,3,4,5,6,7,8-octahydro-1-(methoxyphenyl)methylisoquinoline to the solvent is 1:8-15.
[0026] The molar ratio of the 1,2,3,4,5,6,7,8-octahydro-1-(methoxyphenyl)methylisoquinoline to formaldehyde i...
Embodiment 1
[0032] Put 300g of ethanol into the hydrogenation kettle, add 40g (0.16mol) of 1,2,3,4,5,6,7,8-octahydro-1-(methoxyphenyl)methylisoquinoline, and add it under mechanical stirring 22g (0.22mol) of 30% formaldehyde solution was continuously stirred at 25°C for 4 hours, 6g of Raye's nickel catalyst was added, the hydrogen pressure was 1.8MPa, and stirred at room temperature for 8 hours, the catalyst was removed by filtration, the filtrate was concentrated, separated by vacuum distillation, and 1-( 4-methoxy-benzyl)-2-methyl-1,2,3,4,5,6,7,8-octahydroisoquinoline, yield 90%.
Embodiment 2
[0034] Put 800g of ethanol into the hydrogenation kettle, add 80g (0.32mol) of 1,2,3,4,5,6,7,8-octahydro-1-(methoxyphenyl)methylisoquinoline, and add it under mechanical stirring 44g (0.44mol) of 30% formaldehyde solution was continuously stirred at 30°C for 6 hours, 12g of Raye’s nickel catalyst was added, the hydrogen pressure was 1.5MPa, and stirred at room temperature for 8 hours, the catalyst was removed by filtration, the filtrate was concentrated, and vacuum distillation separated to obtain 1-( 4-methoxy-benzyl)-2-methyl-1,2,3,4,5,6,7,8-octahydroisoquinoline, yield 90.5%.
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