反应详情

A mixture of 3-(tert-butoxycarbonyl)-7-cyano-2,3,4,5-tetrahydro-1H-3-benzazepine (765 mg, 2.81 mmol) and trifluoroacetic acid (2 ml), in dichloromethane (20 ml) was stirred at 40° C. for 1 h. The reaction mixture was evaporated to dryness in vacuo and partitioned between ethyl acetate (50 ml) and water (50 ml). The aqueous layer was basified using potassium carbonate and re-extracted with ethyl acetate (2×30 ml). The combined basic organic extracts were dried over sodium sulfate and evaporated in vacuo to give the title compound as a colourless oil (212 mg, 44%).

1. customThe reaction mixture was evaporated to dryness in vacuo
2. custompartitioned between ethyl acetate (50 ml) and water (50 ml)
3. extractionre-extracted with ethyl acetate (2×30 ml)
4. dry with materialThe combined basic organic extracts were dried over sodium sulfate
5. customevaporated in vacuo