HRID376314

反应详情

EQUATION

反应方程式

HRID 376314 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 16.6 g of thieno[2,3-c]pyridine-N-oxide in 500 ml of chloroform was added 25 g of p-toluenesulfonyl chloride portionwise with ice-cooling over a period of 1 hour. After the reaction mixture was stirred for further 30 minutes under the same conditions, 250 ml of 10% ammonia water was added, and stirred at ambient temperature for 16 hours. The reaction mixture was diluted with 400 ml of chloroform, washed with water and saturated saline, and dried over anhydrous magnesium sulfate. The drying agent was removed by filtration, and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel to give 2.8 g of the title compound as a brown oily material.

WORKUP

后处理

  1. temperaturecooling over a period of 1 hour
  2. additionwas added
  3. washwashed with water and saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe drying agent was removed by filtration
  6. customthe solvent was removed under reduced pressure
  7. customThe residue was purified by column chromatography on silica gel