反应详情

4-(Bicyclo[3.2.1]oct-2-en-2-yl)-3-methyl-benzoic acid of Step B (0.132 g, 0.545 mmol) and 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine (0.111 g, 0.6 mmol) were reacted by in the manner of Example 15, Step D. Purification by flash column chromatography on silica gel, eluting with 20% ethyl acetate in hexane, followed by recrystallization from 1:1 ethyl acetate/petroleum ether afforded the title compound (0.152 g) as white crystals, m.p. 168–169° C.

1. customPurification by flash column chromatography on silica gel
2. washeluting with 20% ethyl acetate in hexane
3. customfollowed by recrystallization from 1:1 ethyl acetate/petroleum ether