HRID1381136

反应详情

EQUATION

反应方程式

HRID 1381136 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(2,4-Dichlorophenyl)-1-mercapto-3-(1H-1,2,4-triazol-1-yl)-propan-2-ol (0.304 g) was stirred in tetrahydrofuran (5 ml) whilst sodium hydride (58 mg of a 50% dispersion in oil, 1.2 equiv.) was added in one portion. After stirring a further five minutes, N-(chloro-methylsulphonyl)piperidine (0.296 g, 1.1 equiv.) was added and heated under reflux for 3 hours. The reaction mixture was allowed to cool to room temperature then poured into an ice/water mixture (20 ml), and extracted with ethyl acetate (3×15 ml). The organic extracts were combined, dried (Na2SO4) and evaporated to a gum, 0.71 g.

WORKUP

后处理

  1. additionwas added in one portion
  2. temperatureheated
  3. temperatureunder reflux for 3 hours
  4. extractionextracted with ethyl acetate (3×15 ml)
  5. dry with materialdried (Na2SO4)
  6. customevaporated to a gum, 0.71 g