Ethanol → HCID 86628834, compound

Participants

Reaction Steps

A stirred mixture of N-(1,3-dimethyl-1H-pyrazol-4-yl)-2-[2-methoxy-4-(7-methoxyquinolin-4-yloxy)phenyl]acetamide (1 g), ethyl acetate (16 ml) and ethanol (4 ml) was heated to reflux until a solution was obtained. The resultant solution was stirred and methanesulphonic acid (0.15 ml) was added dropwise. A precipitate started to form which was dissolved by the addition of ethanol (6 ml). Sufficient ethyl acetate was added until a slightly cloudy solution was formed. The resultant solution was filtered whilst hot and the filtrate was allowed to cool to ambient temperature. The mixture was allowed to stand at ambient temperature for 16 hours. The precipitate was collected by filtration and dried to constant weight under vacuum (1.3×10−4 atmospheres) at 50° C. during 24 hours. There was thus obtained the title salt (1 g); m.p. onset of melting at about 194° C. and a melting point peak at 206-213° C.; 1H NMR: (DMSOd6, at 24° C.) 2.13 (s, 3H), 2.31 (s 3H), 3.68 (s, 2H), 3.7 (s, 3H), 3.79 (s, 3H), 4.04 (s, 3H), 6.88 (d, 1H), 6.95 (m, 1H), 7.11 (d, 1H), 7.42 (d, 1H), 7.53 (d, 1H), 7.58 (m, 1H), 7.8 (s, 1H), 8.48 (d, 1H), 8.94 (d, 1H), 9.46 (s, 1H);

Provenance & Evidence