HRID127513

反应详情

EQUATION

反应方程式

HRID 127513 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 2-indolinthione (7.45 g) in acetone (75 ml) is added potassium carbonate (7.60 g). After stirring, 4-chloro-2-butyn-1-ol (5.48 g) is added thereto. The mixture is stirred at room temperature for 5 hours and filtered. The filtrate is condensed to remove the acetone completely. The residue is dissolved into diethylamine (10 ml), kept at room temperature for 1 hour and evaporated to remove the diethylamine aiming to remove excessive agents. The residue is dissolved in ether (250 ml), washed with water, 2 N hydrochloric acid, water and a saturated saline solution successively, dried and evaporated to give the title compound as an oil (12.0 g).

WORKUP

后处理

  1. stirringThe mixture is stirred at room temperature for 5 hours
  2. filtrationfiltered
  3. customcondensed
  4. customto remove the acetone completely
  5. dissolutionThe residue is dissolved into diethylamine (10 ml)
  6. customevaporated
  7. customto remove the diethylamine aiming
  8. customto remove excessive agents
  9. dissolutionThe residue is dissolved in ether (250 ml)
  10. washwashed with water, 2 N hydrochloric acid, water
  11. customa saturated saline solution successively, dried
  12. customevaporated