HRID1469198

反应详情

EQUATION

反应方程式

HRID 1469198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of (3-methylthiophen-2-yl)(4-propylphenyl)methanone (44, 1.12 g, 4.58 mmol) in acetic acid (4.67 mL) was added pyridinium tribromide (3.67 g, 11.5 mmol). The reaction mixture was heated to 50° C. for 3 hours. After cooling to room temperature, the mixture was poured into water (50 mL) and extracted with EtOAc (100 mL). The organic phase was dried over MgSO4 and evaporated under vacuum. The residue was further purified by silica column chromatography (Biotage) to provide (5-bromo-3-methylthiophen-2-yl)(4-propylphenyl)methanone (45, 0.95 g, 2.95 mmol, 64%).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with EtOAc (100 mL)
  3. dry with materialThe organic phase was dried over MgSO4
  4. customevaporated under vacuum
  5. customThe residue was further purified by silica column chromatography (Biotage)