Diethyl Ether → HCID 22220793, compound

Participants

Reaction Steps

O-(Mesitylenesulfonyl)hydroxylamine containing ca. 18% water (3.03 g, 2.56 g dry wt., ca. 11.9 mmole) was dissolved in dichloromethane (15 mL) and dried over Na2SO4 and filtered. This was added dropwise to a solution of 2-amino-4,6-dimethylpyrimidine (1 g, 8.12 mmole) in 1:6 methanol-dichloromethane (10.5 mL) in an ice bath with stirring. Stirring was continued at 4 C. overnight. Ether (20 mL) was added and the mixture was stirred at 4 C. for 3 hr. The crude product was filtered out and dried (2.50 g). This was dissolved in a minimum amount of methanol, filtered and reduced in volume to 10 mL under reduced pressure. The solution was diluted with dichloromethane (15 mL) and then with ether (15 mL). After stirring at room temp. for 2 hr, the title compound was collected as crystal flakes and dried (2.26 g, mp 242-243 C.).

Provenance & Evidence