反应详情

Boil 15.5 g of 2-(α-ethoxycarbonyl-4-chlorobenzylidene)- 1-methylperhydroazepine and 110 ml of concentrated hydrochloric acid under reflux until the evolution of CO2 ceases. Cool the resulting reaction mixture to ambient temperature; then alkalize it with caustic soda solution (while cooling with ice) and extract the product with diethyl ether. Concentrate the ether phase and dry the prepared concentrate over sodium sulfate. Dissolve the residual 2-(4-chlorobenzylidene)-1-methylperhydroazepine (7.44 g) in ethyl alcohol and hydrogenate with platinum/active carbon/hydrogen. Filter the catalyst from the hydrogenated product, distil off the solvent and then distil the remainder under a high vacuum to obtain 4.4 g of the title compound with a BP of 102° to 110° at 0.003 mm of Hg.

1. temperatureCool
2. customthe resulting reaction mixture to ambient temperature
3. extractionextract the product with diethyl ether
4. concentrationConcentrate the ether phase
5. customdry the prepared
6. concentrationconcentrate over sodium sulfate
7. dissolutionDissolve the residual 2-(4-chlorobenzylidene)-1-methylperhydroazepine (7.44 g) in ethyl alcohol
8. filtrationFilter the catalyst from the hydrogenated product
9. customdistil off the solvent
10. customdistil the remainder under a high vacuum