反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The 6-(t-butyldimethylsilyloxy)-1-[(4-chlorophenyl)sulfonyl]-1-(2,5-difluorophenyl)-2-hexanol (Isomer 234-B) (120 mg, 0.231 mmol) obtained in Example 234 was dissolved in tetrahydrofuran (5 ml), followed by the addition of hydrogen fluoride-pyridine (0.5 ml). The resulting mixture was stirred at room temperature for 20 hours. The reaction mixture was diluted with ethyl acetate, 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. The solid thus obtained was recrystallized from ethyl acetate-hexane, whereby the title compound (51.3 mg, 0.127 mmol, 55%) was obtained as a white powder.
WORKUP
后处理
- washwashed successively with water
- dry with materiala saturated aqueous solution of sodium bicarbonate, and brine, dried over magnesium sulfate
- concentrationconcentrated
- customThe residue thus obtained
- concentrationethyl acetate=1:1 eluate was concentrated
- customThe solid thus obtained