HRID2198050

反应详情

EQUATION

反应方程式

HRID 2198050 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-bromo-5-(trifluoromethyl)aniline (10 g) in pyridine (50 ml) was added methanesulfonyl chloride (5.73 g) at 0° C., and the mixture was stirred at room temperature for 16 hr. The reaction mixture was concentrated, saturated aqueous sodium hydrogencarbonate solution was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with 1M hydrochloric acid and saturated brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated to give the title compound (13.4 g, yield quant.) as a pale-yellow solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additionsaturated aqueous sodium hydrogencarbonate solution was added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with 1M hydrochloric acid and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated