HRID431983

反应详情

EQUATION

反应方程式

HRID 431983 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 4-Iodo-1-trityl-1H-imidazole (5.0 g, 11.6 mmol) in dichloromethane (100 ml) added Ethylmagnesium bromide (3M in diethyl ether) (4.6 ml, 13.9 mmol). Stirred the reaction under argon atmosphere at room temperature for 1 h. At this point added tributyltin chloride (4.1 ml, 13.9 mmol) to the reaction mixture and left the resulting mixture stirring at room temperature overnight. The reaction mixture was diluted with dichloromethane (100 ml), successively washed with saturated ammonium chloride (100 ml), water (100 ml) and brine (100 ml). The organic phase was dried (sodium sulfate), filtered and concentrated in-vacuo to yield 4-Tributylstannyl-1-trityl-1H-imidazole (2.35 g) as a white waxy solid.

WORKUP

后处理

  1. customthe reaction under argon atmosphere at room temperature for 1 h
  2. waitleft the resulting mixture
  3. stirringstirring at room temperature overnight
  4. washsuccessively washed with saturated ammonium chloride (100 ml), water (100 ml) and brine (100 ml)
  5. dry with materialThe organic phase was dried (sodium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated in-vacuo