反应详情

A suspension of 7.7 g (0.040 mol) of 5-chloromethyl-2-methyl-pyrimidin-4-ylamine hydrochloride in 6 ml of dimethyl-formamide was treated with 15 g (0.11 mol) of dry potassium carbonate. At the same time a suspension of 10 g (0.040 mol) of 1-o-tolyl-piperazine dihydrochloride was treated with 15 g (0.11 mol) of dry potassium carbonate in 60 ml of dimethylformamide. After stirring at room temperature for 1/2 hr both solutions were combined and stirred for a further 4 hours. The reaction mixture was suction filtered, the residue was chromatographed over silica gel with dichloromethane/ethyl acetate 1:1 as the eluent and recrystallized from ethanol/ethyl acetate. 2.5 g of 2-methyl-5-(4-o-tolyl-piperazin-1-ylmethyl)-pyrimidin-4-ylamine were obtained as beige crystals; m.p. 189°-190°.

1. stirringstirred for a further 4 hours
2. filtrationfiltered
3. customthe residue was chromatographed over silica gel with dichloromethane/ethyl acetate 1:1 as the eluent
4. customrecrystallized from ethanol/ethyl acetate