反应详情

In dichloromethane (4 ml) was dissolved t-butyl N-[5-[(4-chlorophenyl)sulfonyl]-5(2,5-difluorophenyl)pentyl]-N-methylsulfonylcarbamate (108 mg, 0.196 mmol), followed by the addition of trifluoroacetic acid (1 ml) at room temperature. The resulting mixture was stirred at room temperature for 3 hours. The reaction mixture was diluted with dichloromethane, washed successively with water, a saturated aqueous solution of sodium bicarbonate, and brine, dried over magnesium sulfate and then concentrated. The residue thus obtained was subjected to flash chromatography on a silica gel column, and the fraction obtained from the hexane:ethyl acetate=1:1 eluate was concentrated, whereby the solid thus obtained was recrystallized from ethyl acetate-hexane, whereby the title compound (75.5 mg, 0.167 mmol, 85%) was obtained as a white powder.

1. washwashed successively with water
2. dry with materiala saturated aqueous solution of sodium bicarbonate, and brine, dried over magnesium sulfate
3. concentrationconcentrated
4. customThe residue thus obtained
5. concentrationethyl acetate=1:1 eluate was concentrated
6. customwhereby the solid thus obtained