HRID1958754

反应详情

EQUATION

反应方程式

HRID 1958754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 5-bromo-2-methoxypyrimidine (500 mg, 2.7 mmol) in ethyl acetate (2 mL) and water (0.2 mL) was added trimethylsilylethane (0.41 mL, 3 mmol), triethylamine (0.75 mL, 5.4 mmol), copper iodide (25 mg, 0.13 mmol) and bis(triphenylphosphine)palladium(II) dichloride (47 mg, 0.067 mmol). The solution was heated to 60° C. for 16 h. Ethyl acetate (100 mL) was added and the solution was washed with water (3×10 mL), dried over MgSO4 and treated with decolorizing charcoal. Ethyl acetate was removed in vacuo to give the title compound as a clear oil (547 mg, 97%). 1H NMR (400 MHz, CDCl3) δ 8.56 (s, 2H), 4.01 (s, 3H), 0.24 (s, 9H).

WORKUP

后处理

  1. washthe solution was washed with water (3×10 mL)
  2. dry with materialdried over MgSO4
  3. additiontreated with decolorizing charcoal
  4. customEthyl acetate was removed in vacuo