HRID660724

反应详情

EQUATION

反应方程式

HRID 660724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of n-BuLi (2.5M in hexane, 6.0 mL, 15 mmol) in ether (60 mL) at −78° C. is added a solution of 2-(trimethylsilyl)thiazole (2.0 mL, 12.5 mmol) in ether (20 mL) dropwise. The mixture is stirred at −78° C. for 1 h then tributyltin chloride (4.04 mL, 15 mmol) in ether (25 mL) is added dropwise and stirring is continued at −78° C. for 1 h. The reaction mixture is washed with saturated NaHCO3, dried over anhydrous MgSO4 and concentrated to afford the title compound as a yellow oil which used in the next step without further purification: 1H NMR (CDCl3) δ 0.41 (s, 9H), 0.90 (t, J=8 Hz, 9H), 1.14 (q, 6H), 1.13 (q, 6H), 1.54 (m, 6H), 8.06 (s, 1H); (M+1)+=447.

WORKUP

后处理

  1. stirringstirring
  2. waitis continued at −78° C. for 1 h
  3. washThe reaction mixture is washed with saturated NaHCO3
  4. dry with materialdried over anhydrous MgSO4
  5. concentrationconcentrated