反应详情

The solution of 1.36 g of 3-acetonyl-4-(3-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone, 0.52 g of pyrrolidine and 0.1 g of p-toluenesulfonic acid hydrate in 10 ml of benzene is refluxed with water separation for 4 hours and evaporated. The residue is dissolved in 15 ml of ethanol and the solution hydrogenated over 0.1 g of platinum oxide at atmospheric pressure and room temperature. The mixture is filtered, the filtrate evaporated and the resulting oil dissolved in 2 N hydrochloric acid. The solution is washed with benzene, basified with 3 N aqueous sodium hydroxide and extracted with diethyl ether. The extract is dried, evaporated and the residue recrystallized from petroleum ether and hexane, to yield the 3-(2-pyrrolidinopropyl)-4-(3-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone melting at 94° to 96°.

1. customevaporated
2. dissolutionThe residue is dissolved in 15 ml of ethanol
3. customhydrogenated over 0.1 g of platinum oxide at atmospheric pressure and room temperature
4. filtrationThe mixture is filtered
5. customthe filtrate evaporated
6. dissolutionthe resulting oil dissolved in 2 N hydrochloric acid
7. washThe solution is washed with benzene
8. extractionextracted with diethyl ether
9. customThe extract is dried
10. customevaporated
11. customthe residue recrystallized from petroleum ether and hexane