HRID1877005
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 mixture of methyl 4-[cyclohexyl(5-cyclohexyl-2-ethylthiophen-3-yl)methoxy]benzoate (560 mg) synthesized above, tetrahydrofuran (10 mL) and ethanol (10 mL) was added 1N aqueous sodium hydroxide solution (5 mL), and the mixture was stirred with heating under reflux overnight. The reaction mixture was concentrated under reduced pressure, 1N hydrochloric acid was added, and the mixture was extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate and concentrated under reduced pressure to give a white solid. The obtained solid was recrystallized from ethyl acetate-hexane to give the title compound (194 mg, 36%) as a colorless crystal.
WORKUP
后处理
- temperaturewith heating
- temperatureunder reflux overnight
- concentrationThe reaction mixture was concentrated under reduced pressure, 1N hydrochloric acid
- additionwas added
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto give a white solid
- customThe obtained solid was recrystallized from ethyl acetate-hexane