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 ethyl [2-(5-{[6-(methylsulfonyl)pyridin-3-yl]oxy}-1H-indol-2-yl)-4,5-dihydro-1,3-thiazol-5-yl]acetate (4 g) in ethanol (50 mL) and tetrahydrofuran (50 mL) was added 1N aqueous sodium hydroxide solution (17.4 mL), and the mixture was stirred at room temperature for 15 hr. The reaction mixture was concentrated, and water was added to the residue, and the mixture was washed with ethyl acetate. To the aqueous layer was added 1N hydrochloric acid for neutralization, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure, and crystallized from ethyl acetate and diethyl ether to give the title compound (2.2 g, yield 59%) as yellow powder.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- additionwater was added to the residue
- washthe mixture was washed with ethyl acetate
- additionTo the aqueous layer was added 1N hydrochloric acid for neutralization
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customcrystallized from ethyl acetate and diethyl ether