反应详情

A 3 g. portion of 1-phenyl-3-azabicyclo[3.1.0]hexane hydrochloride is added to a cold (0° C.) mixture of 2.8 g. of acetyl chloride and 6.9 g. of aluminum chloride in 30 ml. of dichloromethane, and the reaction is stirred for 15 minutes. The mixture is then brought to room temperature, stirred overnight and carefully poured onto ice. This mixture is extracted twice with dichloromethane, and the extracts are combined, dried, filtered and concentrated to an oil. This oil is dissolved in a minimum of dichloromethane and treated with an excess of ether to give a solid which is collected, washed with ether and dried. Recrystallization from acetonitrile gives 500 mg. of the desired product, m.p. 195°-197° C.

1. customis then brought to room temperature
2. additioncarefully poured onto ice
3. extractionThis mixture is extracted twice with dichloromethane
4. customdried
5. filtrationfiltered
6. concentrationconcentrated to an oil
7. dissolutionThis oil is dissolved in a minimum of dichloromethane
8. additiontreated with an excess of ether
9. customto give a solid which
10. customis collected
11. washwashed with ether
12. customdried
13. customRecrystallization from acetonitrile
14. customgives 500 mg