反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 0.14 g (0.00086 mol) of 1-phenyl-piperazine in 10 ml of tetrahydrofuran was treated with 0.6 ml (0.0043 mol) of triethylamine and 0.24 g (0.00086 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. 0.14 g (57%) of 5-(4-phenyl-piperazin-1-ylmethyl)-pyrimidine-2,4-diamine was obtained as white crystals; m.p. 263°-265°. A further 0.04 g of yellowish crystals was recovered from the mother liquor.
WORKUP
后处理
- customThe suspension obtained
- filtrationfiltered
- customThe residue was chromatographed over silica gel with acetonitrile/methanol 1:1 as the eluent and digested in diethyl ether