HRID9764

反应详情

EQUATION

反应方程式

HRID 9764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixture of 2-methylthio-4-hydroxy-5-iodopyrimidine (2.65 g), 3-phenyl-1-propyne (1.49 mL), copper (I) iodide (90 mg) and bis(triphenylphosphine) Palladium (II) dichloride (Fluka, 160 mg) in 20 mL of triethylamine and NMP (7 mL) was stirred at 40° C. for 6 hours. The reaction mixture was diluted with ethyl acetate (100 mL), washed with brine (3×50 mL), concentrated and purified by column chromatography (5% EtOAc/hexanes) to give 0.57 g of a solid product. MP: 69–72.2° C. MS: 257.2 (M+H).

WORKUP

后处理

  1. washwashed with brine (3×50 mL)
  2. concentrationconcentrated
  3. custompurified by column chromatography (5% EtOAc/hexanes)