tert-Butyl methyl ether → HCID 86628835, compound

Participants

Reaction Steps

A stirred suspension of N-(1,3-dimethyl-1H-pyrazol-4-yl)-2-[2-methoxy-4-(7-methoxyquinolin-4-yloxy)phenyl]acetamide (0.605 g) in ethanol (5 ml) was heated to reflux until a solution was obtained. The resultant solution was stirred and a solution of 4-toluenesulphonic acid monohydrate (0.333 g; 1.25 equivalents) in ethanol (95%, 5 ml) was added. The mixture was allowed to start to cool and tert-butyl methyl ether (12 ml) was added. The resultant mixture was allowed to stand at ambient temperature for 29 hours. The precipitate was collected by filtration and dried to constant weight under vacuum (1.3×10−4 atmospheres) at 50° C. during 4 hours. There was thus obtained the title salt (0.705 g); m.p. 126-136° C.; 1H NMR: (DMSOd6, at 24° C.) 2.13 (s, 3H), 2.28 (s, 3H), 3.68 (s, 2H), 3.7 (s, 3H), 3.79 (s, 3H), 4.03 (s, 3H), 6.87 (d, 1H), 6.95 (m, 1H), 7.08-7.13 (m, 3H), 7.42 (d, 1H), 7.47 (d, 2H), 7.51 (d, 1H), 7.58 (m, 1H), 7.8 (s, 1H), 8.47 (d, 1H), 8.93 (d, 1H), 9.46 (s, 1H);

Provenance & Evidence