Hydrochloric Acid → HCID 135800602, compound

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A mixture of 8-amino-1,3,5-trimethyl-1H-pyrimido-{4,5-c}-1,2-diazepin-6(7H)-one (219 mg) and N hydrochloric acid (3 ml) was heated using a hot water bath (>85° C.) for 2 hours. During that period a solution formed before crystals gradually began to separate. The mixture stood at room temperature overnight before the straw-coloured crystals were collected, washed with water and dried under vacuum (70° C.) to yield 140 mg (78%) of analytically pure product: mp >300°; nmr (DMSO-d6) δ 2.28 (s, 3H), 3.60 (s, 3H), 6.52 (br s, 2H), 10.30 (br s, 1H); uv λ max (CH3OH) 217 nm (ε 26,800), 254 (13,000). Mass spectrum (120° C., 70 ev): M, m/e 179, 100%.

Provenance & Evidence