反应详情

Trifluoromethanesulfonic anhydride (5.6 mL) is added dropwise to a solution of 2,2,2-trifluoro-1-(cis-6-hydroxy-2,3,4,4a,9,9a-hexahydro-indeno[2,1-b]pyridin-1-yl)-ethanone (7.3 g), triethylamine (7.2 mL), and 4-dimethylaminopyridine (50 mg) in dichloromethane (60 mL) chilled in an ice bath. The solution is stirred with cooling for 1 h and at room temperature for 2 h. Water (100 mL) and dichloromethane (100 mL) are then added and the organic phase is separated. The organic phase is washed with water (50 mL), dried (MgSO4), and concentrated to give the title compound as a dark oil. Yield: 10.7 g (quantitative); TLC: rf=0.50 (silica gel, cyclohexane/ethyl acetate 3:1); Mass spectrum (ESI+): m/z=418 [M+H]+.

1. temperaturechilled in an ice bath
2. customthe organic phase is separated
3. washThe organic phase is washed with water (50 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated