HRID2252069

反应详情

EQUATION

反应方程式

HRID 2252069 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add thioacetamide (0.09 g, 1.2 mmol) to a solution of 2-bromoacetophenone (0.2 g, 1.0 mmol) in 30 mL dioxane. Stir at room temperature for 4 hours, dilute with ethyl acetate, wash sequentially with aqueous sodium carbonate (3×15 mL) and water (3×20 mL). Dry the organic phase over sodium sulfate, concentrate under reduced pressure, and subject the residue to silica gel chromatography, eluting with hexane containing 10% ethyl acetate to provide the desired compound in 78% yield. MS(ES+): m/z=176.1 (M+H)+

WORKUP

后处理

  1. washwash sequentially with aqueous sodium carbonate (3×15 mL) and water (3×20 mL)
  2. dry with materialDry the organic phase over sodium sulfate
  3. concentrationconcentrate under reduced pressure
  4. washeluting with hexane containing 10% ethyl acetate