HRID2294041

反应详情

EQUATION

反应方程式

HRID 2294041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8.0 g (0.031 mol) of 1-(2-chloro-phenyl)-piperazine in 300 ml of tetrahydrofuran was treated with 22 ml (0.16 mol) of triethylamine and 11.5 g (0.031 mol) of 5-bromomethyl-pyrimidine-2,4-diamine dihydrobromide and the mixture was stirred at room temperature under argon for 16 hours. The suspension obtained was suction filtered and the filtrate was completely freed from the solvents. The residue was chromatographed over silica gel with acetonitrile/methanol 1:1 as the eluent and digested in diethyl ether. 5.5 g (55%) of 5-[4-(2-chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine were obtained as beige crystals; m.p. 2:30°-235°.

WORKUP

后处理

  1. customThe suspension obtained
  2. filtrationfiltered
  3. customThe residue was chromatographed over silica gel with acetonitrile/methanol 1:1 as the eluent and digested in diethyl ether