HRID2220116

反应详情

EQUATION

反应方程式

HRID 2220116 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

n-Butyllithium (1.6M, 4.95 mL, 7.88 mmol) was added to a solution of 2-trimethylsilylthiazole (826 mg, 5.25 mmol) in anhydrous ether (45 mL) stirred at −78° C. under nitrogen. After 20 min, tri-n-butylstannyl chloride (2.57 g, 7.88 mmol) was added, then the solution was allowed to warm to room temperature, and stirred for another 1 h. The mixture was quenched and washed with 1N sodium hydroxide, dried through MgSO4, and then the solvent was evaporated to give a brown oily residue. The residue of 2-trimethylsilyl-5-tributylstannyl-thiazole was passed through a column of neutral alumina eluting with a gradient of ammoniated methanol in chloroform to give the sub-title compound as a yellow oil (1.5 g).

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. stirringstirred for another 1 h
  3. customThe mixture was quenched
  4. washwashed with 1N sodium hydroxide
  5. dry with materialdried through MgSO4
  6. customthe solvent was evaporated
  7. customto give a brown oily residue