HRID1482649

反应详情

EQUATION

反应方程式

HRID 1482649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-methoxyl-1-(4-chlorobutyl)-1H-benzotriazole (0.06 mol) was dissolved into 150 ml of acetonitrile, 4-(3-(3-trifluoromethylphenyl) piperidine (0.05 mol), diisopropylethylamine (0.2 mol) and potassium iodide (0.05 mol) were respectively added. The mixture was stirred for 10 min at ambient temperature, and then heated and refluxed to react for 15 hours. The mixture was cooled down to ambient temperature and filtered. The filtrate was concentrated to produce oily products, and treated by chromatography with neutral Al2O3, purified, eluted with dichloromethane/methanol mixture to produce 14.0 g N-(4-(1H-benzotriazole-1-yl)butyl)-4-(3-trifluoromethylphenyl)piperidine (I-131) with a yield of 64.6%. ESI-MS [M+H]+: m/z 433.2.

WORKUP

后处理

  1. temperatureheated
  2. temperaturerefluxed
  3. customto react for 15 hours
  4. temperatureThe mixture was cooled down to ambient temperature
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated
  7. customto produce oily products
  8. additiontreated by chromatography with neutral Al2O3
  9. custompurified
  10. washeluted with dichloromethane/methanol mixture