反应详情

A 500 mL round bottom flask equipped with a magnetic stir bar was charged with 1,1-dimethylethyl{cis-4-[({[2(trifluoromethyl)phenyl]methyl}amino)carbonyl]cyclohexyl}carbamate (24.88 g, 62.1 mmol) and dichloromethane (100 mL). Trifluoroacetic acid (100 mL) was added slowly, and the reaction mixture was stirred at room temperature for 1 h. The volatile components were removed by rotary evaporation, and the crude oil was dissolved in ethyl acetate and washed with saturated sodium bicarbonate solution (3×200 mL). The organic phase was dried over Na2SO4, filtered and concentrated to give 18.3 g of the title compound (98%) as an off-white solid. MS (ES) m/e 301 [M+H]+.

1. customA 500 mL round bottom flask equipped with a magnetic stir bar
2. customThe volatile components were removed by rotary evaporation
3. dissolutionthe crude oil was dissolved in ethyl acetate
4. washwashed with saturated sodium bicarbonate solution (3×200 mL)
5. dry with materialThe organic phase was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated