HRID1161742

反应详情

EQUATION

反应方程式

HRID 1161742 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Aqueous potassium phosphate was added to a suspension of 2,4-dimethylbenzene boronic acid and 2-amino-4,6-dichloro-5-pyrimidinecarbaldehyde (3 eq) in 1,4-dioxan, under a nitrogen atmosphere. Dichloro bis(triphenylphosphine)palladium (II) (cat.) was added and the mixture heated, ˜100° C., for ˜90 mins. The resulting mixture was allowed to cool and dichloromethane added, the mixture was washed with water and saturated aqueous sodium chloride solution. The solution was dried over anhydrous sodium sulphate and concentrated to a pale yellow solid. The crude solid was purified by column chromatography on silica eluting with mixtures of diethyl ether and hexane.

WORKUP

后处理

  1. temperatureto cool
  2. washthe mixture was washed with water and saturated aqueous sodium chloride solution
  3. dry with materialThe solution was dried over anhydrous sodium sulphate
  4. concentrationconcentrated to a pale yellow solid
  5. customThe crude solid was purified by column chromatography on silica eluting with mixtures of diethyl ether and hexane