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ChemicalBook CAS DataBase List 4-Pyrimidinamine, 6-methoxy-N-methyl- (9CI)

4-Pyrimidinamine, 6-methoxy-N-methyl- (9CI) synthesis

3synthesis methods
-

Yield:1124-73-8 95%

Reaction Conditions:

in methanol; for 96 h;Reflux;

Steps:

23 PREPARATION 236-Methoxy-N-methylpyrimidin-4-amine

The title compound of PREPARATION 22 (8.5 g, 59 mmol) was dissolved in 100 ml methanol. Sodium methoxide (19.8 g, 370 mmol) was added in several portions over a4 day period while the mixture was stirred at reflux. The mixture was allowed to cool and was evaporated under reduced pressure. The solid residue was resuspended in dichloromethane and was stirred for 1 h. The solution was filtered and the filtrate was evaporated under reduced pressure to give 7.80 g (56 mmol, 95% yield) of the title compound as a white solid. Purity 100%.1H NMR (300 MHz, DMSO-d6) ? ppm 8.10 (s, 1H), 7.00 (s, 1H), 5.62 (s, 1H), 3.80 (s,3H), 3.10 (s, 3H)UPLC/MS (3 mm) retention time 0.45 mm.LRMS: m/z 140 (M+1).

References:

WO2017/64068,2017,A1 Location in patent:Page/Page column 41