HRID370564

反应详情

EQUATION

反应方程式

HRID 370564 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 1-trichloromethyl-3-methyl-2-butenyl acetoacetate (0.575 g, 2 mmole) and triethylamine (0.404 g, 4 mmole) in 10 ml of acetonitrile was added 1 g of polymer-bound sulfonyl azide (prepared by the method of Roush, et al., loc. cit.). The mixture was stirred overnight at room temperature and filtered. The filter cake was washed with ether, and the slurry was filtered. Solvent was removed by evaporation from the combined filtrates to give 1-trichloromethyl-3-methyl-2-butenyl 2-diazoacetoacetate (0.60 g, 96% yield).

WORKUP

后处理

  1. customprepared by the method of Roush, et al., loc
  2. filtrationfiltered
  3. washThe filter cake was washed with ether
  4. filtrationthe slurry was filtered
  5. customSolvent was removed by evaporation from the combined filtrates