HRID1975662

反应详情

EQUATION

反应方程式

HRID 1975662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

To a solution of 1.0 g of 2-butyl-6-iodo-4(1H)-quinazolinone 0.043 g of bis(triphenylphosphine) palladium (II) chloride and 5.8 mg of copper (I) iodide in 5.0 ml of N,N-dimethylformamide and 5.0 ml of triethylamine is added 0.36 g of (trimethylsilyl) acetylene. The resulting reaction mixture is heated at 45° C. for 1 hour and then 65° C. for 5 hours. Upon cooling, the reaction mixture is concentrated in vacuo and the residue purified by flash chromatography on silica gel, eluting with 1:3 ethyl acetate-hexane to yield 0.75 g of the desired product as a white solid. CI MASS SPEC 299(MH+).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. temperatureUpon cooling
  3. concentrationthe reaction mixture is concentrated in vacuo
  4. customthe residue purified by flash chromatography on silica gel
  5. washeluting with 1:3 ethyl acetate-hexane