HRID347619

反应详情

EQUATION

反应方程式

HRID 347619 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 3.05 g (15 mMol) of 5-amino-3-(2-dimethylaminoethyl)-1H-indol in 100 ml of pyridine is added dropwise at ambient temperature a solution of 4.21 g (15 mMol) of 5-chloro-3-methyl-benzo[b]thiophene-2-sulphonyl chloride in 20 ml of pyridine. The reaction mixture is stirred at ambient temperature for 20 hours. It is then evaporated to dryness, slightly alkalinised with diluted ammonia and dissolved in ethyl acetate. The organic phase is washed with water and a saturated solution of sodium bicarbonate, it is separated and dried with anhydrous sodium sulphate. The organic solution is evaporated to dryness and the resulting solid is repeatedly washed with ethyl ether, to yield 5.5 g (82%) of N-[3-(2-dimethylaminoethyl)-1H-indol-5-yl]-5-chloro-3-methyl-benzo[b]thiophene-2-sulphonamide as a solid with m.p.=226–227° C.

WORKUP

后处理

  1. customIt is then evaporated to dryness
  2. dissolutiondissolved in ethyl acetate
  3. washThe organic phase is washed with water
  4. customa saturated solution of sodium bicarbonate, it is separated
  5. dry with materialdried with anhydrous sodium sulphate
  6. customThe organic solution is evaporated to dryness
  7. washthe resulting solid is repeatedly washed with ethyl ether