反应详情

A suspension of (3aR*,10aS*)-4-(aminoacetyl)-9-benzyl-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta-[e][1,4]diazepin-10(1H)-one (0.58 g, 1.7 mmol) and 4-chlorophthalic anhydride (0.31 g, 1.7 mmol) in toluene (10 mL) was refluxed for 3.5 hours using a Dean-Stark water separator. The reaction mixture was left standing for cooling at room temperatures, to which was added hexane. The resulting solid was collected by filtration, which was recrystallized from chloroform-hexane to give 0.66 g (yield 75%) of the titled compound, m.p. 237°-238° C.

1. temperaturewas refluxed for 3.5 hours
2. waitThe reaction mixture was left
3. temperaturefor cooling at room temperatures, to which
4. filtrationThe resulting solid was collected by filtration, which
5. customwas recrystallized from chloroform-hexane