反应详情

To a mixture of 1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)piperazine (1.2 g), triethylamine (0.5 g) and methylene chloride (20 ml) is added dropwise, with stirring under ice-cooling, a solution of 3,5-dimethoxy-4-ethoxybenzoyl chloride (1.0 g) in methylene chloride (20 ml). The reaction mixture is then stirred for one hour at room temperature, and then poured into ice-water, followed by extraction with methylene chloride. The organic layer is washed with water, dried and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography (hexane:ethyl acetate:acetone=1:2:1) to afford 1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)-4-(3,5-dimethoxy-4-ethoxy-benzoyl)piperazine (0.9 g). This product is recrystallized from ethyl acetatehexane to give colorless needles, m.p. 171°-172° C.

1. additionis added dropwise
2. temperaturecooling
3. stirringThe reaction mixture is then stirred for one hour at room temperature
4. extractionfollowed by extraction with methylene chloride
5. washThe organic layer is washed with water
6. customdried
7. concentrationconcentrated under reduced pressure
8. customThe concentrate is purified by silica gel column chromatography (hexane:ethyl acetate:acetone=1:2:1)