6-amino-4-chloro-2-methylpyrimidine

A mixture of 2-methyl-4,6-dichloropyrimidine 25.41g (0.1559 mol) and 7M NH3 in anhydrous methanol 260mL was heated in a pressure flask at 110 C for one day. The cooled reaction mixture was evaporated and the obtained solid residue was re-crystallized from water (100mL, at +5C, overnight). The crystallized product (14.587g) was collected by filtration, rinsed with ice-cold water and dried on highvac. A second pure fraction (2.536g) was obtained by concentrating the supernatants to a small volume. Y=17.123g (76.5%) of a white crystalline solid. 1H(d6-DMSO, 400MHz): 7.101(br s, 2H), 6.258(s, 1H), 2.284(s, 3H) 

A mixture of 2-methyl-4-chloro-6-aminopyrimidine 2.532g (17.63 mmol) and N-(2-hydroxyethyl)-piperazine 6.0mL (48.9 mmol) was heated without solvent under Ar at 165 C for 75min. The amine excess was removed on highvac (with heating on oil bath), the solid residue was re-evaporated from a mixture of chloroform-methanol (1:1, 60mL), the oily residue was diluted with chloroform 10mL and allowed to crystallize overnight. The product was collected by quick filtration under Ar blanket, washed with chloroform (2x10mL) and dried on highvac. Y=2.774g (66%) of a white hygroscopic crystalline solid. 1H(d6-DMSO, 400MHz): 6.081(br s, 2H), 5.417(s, 1H), 4.434(br s, 1H), 3.515(app t, 6.0Hz, 2H), 3.380(app br t, 4.8Hz, 4H), 2.413(m, 6H), 2.149(s, 3H)