反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of methyl trans-4-[(4-chlorophenyl) sulfonyl]cyclohexanecarboxylate (209 mg, 0.81 mol) synthesized in (10B) in methanol (10 ml), 2 N sodium hydroxide (0.5 ml, 1 mmol) was added at room temperature, and the resulting mixture was stirred at the same temperature for 1 hour. Then, to the reaction solution, 2 N hydrochloric acid (0.5 ml, 1 mmol) was added, and extraction was performed once with ethyl acetate. The obtained organic layer was washed with water and a saturated aqueous solution of sodium chloride and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:90 to 0:100 (v/v)), whereby the title compound was obtained as an oil (180 mg, yield: 73%).
WORKUP
后处理
- additionwas added at room temperature
- extractionextraction
- washThe obtained organic layer was washed with water
- dry with materiala saturated aqueous solution of sodium chloride and then dried over anhydrous sodium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:90 to 0:100 (v/v)), whereby the title compound