反应详情

To a solution of chloroacetyl chloride (7.0 g) in dichloroethane (50 ml) was added aluminum chloride (8.2 g) at room temperature, and then a solution of 3-(trifluoroacetyl)-2,3,4,5-tetrahydro-1H-3-benzazepine (3.0 g) in dichloroethane (50 ml) was added. The obtained mixture was stirred at room temperature for 3 hr, and poured into ice-cooled 1N is hydrochloric acid (80 ml). Dichloroethane was evaporated under reduced pressure, and the residue was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane (1:1, volume ratio) to give the title compound (3.5 g) as a colorless powder.

1. additionpoured into ice-
2. temperaturecooled 1N
3. customDichloroethane was evaporated under reduced pressure
4. extractionthe residue was extracted with ethyl acetate
5. washThe extract was washed with saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was recrystallized from ethyl acetate-hexane (1:1, volume ratio)