HRID1444180
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
CONDITIONS
反应条件
- 温度
- 180 °C
PROCEDURE
实验过程
Water (2.5 μl, 0.14 mmol) was added to a solution of methyl 2-bromoimidazo[5,1-b]thiazole-7-carboxylate (36 mg, 0.14 mmol) and lithium iodide (73 mg, 0.55 mmol) in dimethyl sulfoxide (8 ml) solution, and the mixture was stirred at 180° C. for 2 hr. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate (5 ml×3). The organic layer was washed with saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1) to give 2-bromoimidazo[5,1-b]thiazole (4.5 mg, 16%) as a white solid.
WORKUP
后处理
- extractionthe mixture was extracted with ethyl acetate (5 ml×3)
- washThe organic layer was washed with saturated brine
- dry with materialwas dried over anhydrous sodium sulfate
- customThe solvent was removed by distillation under the reduced pressure
- customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1)