HRID1444181

反应详情

EQUATION

反应方程式

HRID 1444181 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Concentrated hydrochloric acid (0.3 ml) was added to a solution of methyl 2-bromoimidazo[5,1-b]thiazole-7-carboxylate (54 mg, 0.21 mmol) in propionic acid (2 ml), and the mixture was heated under reflux for 11 hr. The reaction solution was neutralized with a 2 M aqueous solution of sodium hydroxide and was extracted with ethyl acetate (7 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=1:2) to give 2-bromoimidazo[5,1-b]thiazole (12 mg, 28%) as a white solid.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 11 hr
  3. extractionwas extracted with ethyl acetate (7 ml×3)
  4. washThe organic layer was washed with saturated brine
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. customThe solvent was removed by distillation under the reduced pressure
  7. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:2)