HRID1501103

反应详情

EQUATION

反应方程式

HRID 1501103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 5-bromo-2,6-dimethylpyrimidin-4-ol (3.7 g, 18.3 mmol), dicyano zinc (10.7 g, 91.5 mmol) and tetrakis(triphenylphosphine)palladium (6.3 g, 5.1 mmol) and N,N-dimethylformamide (60 mL) was stirred at 140° C. for 12 hours. The mixture was concentrated to give a residue. The residue was purified by column chromatography (silica gel, dichloromethane/methanol=15:1) to give 4-hydroxy-2,6-dimethylpyrimidine-5-carbonitrile as a white solid (2.7 g, 99%). LRMS (M+H) m/z: calcd 149.06. found 149.

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. customto give a residue
  3. customThe residue was purified by column chromatography (silica gel, dichloromethane/methanol=15:1)