HRID1157819

反应详情

EQUATION

反应方程式

HRID 1157819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a stirred solution of tert-butyl 4-(1-cyano-2-phenylvinyl)piperazine-1-carboxylate (100 mg) taken in dry DMSO (2 ml) added sodium azide (0.2 g) and heated to 110° C. overnight. The reaction mixture was carefully quenched with water (10 ml) and the reaction mixture was extracted with dichloromethane (3×10 ml). The combined organic layer was washed with brine (10 ml), dried over sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by column chromatography using MeOH: CH2Cl2 (1:9) as an eluent to afford tert-butyl 4-(5-phenyl-1H-1,2,3-triazol-4-yl)piperazine-1-carboxylate as white solid.

WORKUP

后处理

  1. customThe reaction mixture was carefully quenched with water (10 ml)
  2. extractionthe reaction mixture was extracted with dichloromethane (3×10 ml)
  3. washThe combined organic layer was washed with brine (10 ml)
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by column chromatography