反应详情

7.87 g of N-[2-hydroxy-2-(4-methoxyphenyl)ethyl]-2-(2-chloro-3,4-dimethoxyphenyl)ethylamine was dissolved in 59 ml of CF3COOH. 1.7 ml of concentrated H2SO4 was added to the solution and the reaction was conducted for 4 hours. After the completion of the reaction followed by concentration under reduced pressure, 100 ml of CHCl3 and 50 ml of 10% NaOH were added to the residue to conduct extraction. The extract was washed with water, dehydrated over MgSO4 and concentrated to dryness under reduced pressure to obtain 6.25 g (yield: 83.5%) of 6-chloro-2,3,4,5-tetrahydro-7,8-dimethoxy-1-(4-methoxyphenyl)-1H-3-benzazepine.

1. concentrationAfter the completion of the reaction followed by concentration under reduced pressure, 100 ml of CHCl3 and 50 ml of 10% NaOH
2. additionwere added to the residue
3. extractionextraction
4. washThe extract was washed with water
5. concentrationconcentrated to dryness under reduced pressure