HRID1603540

反应详情

EQUATION

反应方程式

HRID 1603540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Argon is passed through a solution of 200 mg of 6-iodo-4-methoxy-quinazoline in 12 ml of dry dimethylformamide for 15 minutes. Then 40 mg of tetrakis(triphenylphosphine)-palladium, 113 mg of (2,5-dimethoxyphenyl)acetylene, 11 mg of copper(I)iodide and 220 mg of triethylamine are added, and the mixture is heated to 60° for 2 hours. The solvent is distilled off in vacuo and the residue partitioned between water and ethyl acetate. The organic layer is separated, dried and concentrated in vacuo. The pure title compound is obtained after chromatography (silica gel, cyclohexane/ethyl acetate=2/1) as colourless crystals. mp: 103-105°.

WORKUP

后处理

  1. temperaturethe mixture is heated to 60° for 2 hours
  2. distillationThe solvent is distilled off in vacuo
  3. customthe residue partitioned between water and ethyl acetate
  4. customThe organic layer is separated
  5. customdried
  6. concentrationconcentrated in vacuo