1-Piperazineethanol,4-(6-amino-2-methyl-4-pyrimidinyl)- (914347-48-1)

With the CAS registry number 914347-48-1,  2-(4-(6-Amino-2-methylpyrimidin-4-yl)piperazin-1-yl)ethanol is also named as 1-piperazineethanol, 4-(6-amino-2-methyl-4-pyrimidinyl)- . The following is the synthese method:

1. In anhydrous methanol 260mL, a mixture of 2-methyl-4,6-dichloropyrimidine 25.41g (0.1559 mol) and 7M NH₃ was heated in a pressure flask at 110 °C for one day. 2. Cool the reaction mixture and then evaporat, the obtained solid residue was re-crystallized from water (100mL, at +5 °C, overnight). 3. The crystallized product (14.587g) was collected by filtration, rinsed with ice-cold water and dried on highvac. 4. A second pure fraction (2.536g) was obtained by concentrating the supernatants to a small volume. Yield 17.123g (76.5%) of a white crystalline solid. 5. Without solvent, 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 under Ar at 165 C for 75min. 6. With heating on oil bath, the amine excess was removed on highvac. 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. 7. The product was got by quick filtration under Ar blanket, washed with chloroform (2×10mL) and dried on highvac.