HRID1441139

反应详情

EQUATION

反应方程式

HRID 1441139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 2,4,6-trichloropyrimidine (6.9 g) in 75 ml of tetrahydrofuran is treated with diisopropylethylamine (15 ml) and solid taurine (4.7 g). The resulting suspension is heated at reflux for 48 hours. The reaction mixture is cooled to 20°-25° followed by solvent evaporation which gives 26 g of an oil which is chromatographed on 170 g of silica gel and eluting with chloroform/5.0M ammonia in methanol (7/3). An initial fraction of 250 mL is collected followed by 20 ml fractions. Fractions 23-57 contained the desired product. Solvent evaporation gives a semi-solid which is taken up in chloroform/methanol (10/1) and stirred at 20°-25° for 30 minutes. Filtration provided 3.71 g of a solid.

WORKUP

后处理

  1. temperatureThe resulting suspension is heated
  2. temperatureat reflux for 48 hours
  3. temperatureThe reaction mixture is cooled to 20°-25°
  4. customfollowed by solvent evaporation which