HRID1292247

反应详情

EQUATION

反应方程式

HRID 1292247 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of the 4-bromobenzenesulfonamide derivative (1 g, 2.64 mmol) prepared in Step (a) and 4-methoxybenzeneboronic acid (0.48 g, 3.17 mmol) in toluene (10 mL) was treated with tetrakis(triphenylphosphine)palladium(0) (0.15 g, 0.1 mmol) and aqueous sodium carbonate (0.5 g/5 mL H2O), respectively. The reaction mixture was refluxed for 3 hours, then cooled to room temperature. Ethyl acetate (25 mL) and aqueous HCl (1M, 25 mL) were added, the layers separated, and the organic portion was dried (MgSO4), filtered, and the filtrate was concentrated in vacuo. The resulting solid was triturated with hexane/ethyl acetate (3:1) and was collected by filtration. Yield: 0.68 g (62%);

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 3 hours
  2. customthe layers separated
  3. dry with materialthe organic portion was dried (MgSO4)
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated in vacuo
  6. customThe resulting solid was triturated with hexane/ethyl acetate (3:1)
  7. filtrationwas collected by filtration