HRID1363200

反应详情

EQUATION

反应方程式

HRID 1363200 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a suspension of NaOH (4.44 g) in 1,2-dichloroethane (250 mL) was added 4-oxo-4,5,6,7-tetrahydroindole (5.0 g). The mixture was then cooled to 0° C. and stirred for 30 min, following which a solution of phenylsulfonyl chloride (5.7 mL) in 1,2-dichloroethane (50 mL) was added dropwise over a period of 30 min. After 30 min of stirring, the reaction mixture was allowed to come to room temperature and stirred overnight. The reaction was quenched by pouring onto distilled water (100 mL). The organic layer was separated, and the aqueous layer was extracted with dichloromethane (3×50 mL). The combined organic extract was washed with distilled water to neutrality, dried over MgSO4, and concentrated in vacuo to afford 7.0 g of the title compound.

WORKUP

后处理

  1. additionwas added dropwise over a period of 30 min
  2. stirringAfter 30 min of stirring
  3. customto come to room temperature
  4. stirringstirred overnight
  5. customThe reaction was quenched
  6. additionby pouring
  7. distillationonto distilled water (100 mL)
  8. customThe organic layer was separated
  9. extractionthe aqueous layer was extracted with dichloromethane (3×50 mL)
  10. extractionThe combined organic extract
  11. washwas washed with distilled water to neutrality
  12. dry with materialdried over MgSO4
  13. concentrationconcentrated in vacuo