反应详情

A stirred mixture of 5.0 g of 5,6-dimethoxy-3-(4-piperidyl)-1,2-benzisoxazole, 6.78 g of 2-methyl-3-(phenylsulfonylpropyl)indole, 120 ml of dimethylformamide and 15.0 g of anhydrous potassium carbonate was heated to 90° for 6 hrs and overnight at ambient temperature. The mixture was poured into water (300 ml) and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and the solvent was removed in vacuo to yield a solid. The solid was purified by passing it through a silica gel column (20:1) and eluting it with dichloromethane-methanol (1%). Recrystallization two times from ethanol-water yielded 2.0 g (24%) of product, mp 176°-178°.

1. extractionextracted with ethyl acetate
2. dry with materialThe extract was dried over anhydrous magnesium sulfate
3. customthe solvent was removed in vacuo
4. customto yield a solid
5. customThe solid was purified
6. washeluting it with dichloromethane-methanol (1%)
7. customRecrystallization two times from ethanol-water