HRID2388196

反应详情

EQUATION

反应方程式

HRID 2388196 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 4-methyl-3-(pyridin-4-yl)isoxazole-5-carboxylate (5.1 g, 22.0 mmol), NBS (4.7 g, 26.4 mmol), and benzoyl peroxide (0.53 g, 2.2 mmol) were added to 140 mL of carbon tetrachloride and the mixture was refluxed for 16 h. Solvent was removed in vacuo and the crude product was purified by flash chromatography (10-60% EtOAc/hexanes) to afford 1.5 g of the title compound. MS: (+) m/z 311, 313 (M+1, 79Br/81Br).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 16 h
  2. customSolvent was removed in vacuo
  3. customthe crude product was purified by flash chromatography (10-60% EtOAc/hexanes)