HRID429246

反应详情

EQUATION

反应方程式

HRID 429246 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

The 2,6-dichlorobenzylsulfonamide (8 g, 33.47 mmol) was added to potassium carbonate (4.62 g, 33.47 mmol), copper powder (560 milligrams (hereinafter“mg”)) and N,N-dimethylaniline (10 ml) in flask. The reaction mixture was stirred at 170° C. for 4 hours, then it was cooled to room temperature and partitioned between ethyl acetate and 10% aqueous HCl. The combined organic phase was dried and concentrated. Chromatography of the residue on silica gel (30% Ethyl acetate/Hexane) gave desired product (4 g, 59%). MS(EI) m/e 204.5 (M+).

WORKUP

后处理

  1. temperatureit was cooled to room temperature
  2. custompartitioned between ethyl acetate and 10% aqueous HCl
  3. customThe combined organic phase was dried
  4. concentrationconcentrated