HRID1767870
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 4-[4-methyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethoxy]-1H-indole (50 mg, 130 μmol) and bromo-acetic acid tert-butyl ester (20 μl, 140 μmol) in DMF (4 ml) was added sodium hydride (55%, 8 mg, 176 μmol) under an argon atmosphere at 0° C. The mixture was naturally warmed to room temperature, stirred for 72 h, poured onto 1 N HCl/ice water 1/1 and extracted three times with dichloromethane. The combined organic layers were washed with water and dried over sodium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography (silica gel, heptane/AcOEt) to give 50 mg (99 μmol, 77%) of the title compound as light yellow oil.
WORKUP
后处理
- extractionextracted three times with dichloromethane
- washThe combined organic layers were washed with water
- dry with materialdried over sodium sulfate
- customThe solvent was removed under reduced pressure
- customthe residue purified by column chromatography (silica gel, heptane/AcOEt)