HRID1444180

反应详情

EQUATION

反应方程式

HRID 1444180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionthe mixture was extracted with ethyl acetate (5 ml×3)
  2. washThe organic layer was washed with saturated brine
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. customThe solvent was removed by distillation under the reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1)