[CH2:1]([C:3]1[C:4]([O:15][CH3:16])=[N:5][C:6]2[N:7]([CH:10]=[C:11]([C:13]#[N:14])[N:12]=2)[C:8]=1[CH3:9])[CH3:2].C(Cl)(Cl)Cl.[OH2:21]>>[CH2:1]([C:3]1[C:4]([O:15][CH3:16])=[N:5][C:6]2[N:7]([CH:10]=[C:11]([C:13]([NH2:14])=[O:21])[N:12]=2)[C:8]=1[CH3:9])[CH3:2]A suspension of 10.0 g of 6-ethyl-7-methoxy-5-methylimidazo[1,2-a]pyrimidine-2-carbonitrile of Step A and 20.0 g of Amberlite IRA-400 (base form) in 200 ml of water was stirred rapidly at reflux and after 41/2 hours, the mixture was cooled. Chloroform was added to dissolve the precipitated product and the two phase mixture was filtered to remove the Amberlite. The layers were separated and the aqueous phase was extracted with chloroform. The combined chloroform layers were dried over MgSO4, filtered and evaporated to dryness. The solid product was crystallized from methanol to obtain 10.5 g (97% yield) of 6-ethyl-7-methoxy-5-methylimidazo[1,2-a]pyrimidine-2-carboxamide as white needles melting at 256°-259° C.
Wird geladen…