Hydrochloric Acid → HCID 69566254, compound

Participants

Reaction Steps

To a stirred solution of tert-butyl-[4-(3-{5-[(cyclopropylamino)carbonyl]-2-methylphenyl}-4-oxo-3,4-dihydroquinazolin-6-yl)piperazin-1-yl]acetate (0.28 g) in methylene chloride (10 ml) was added 4N HCl in dioxane (3 ml). After 72 hours water (15 ml) was added and the solution poured onto an ion exchange column (isolute SCX-2 column from International Sorbent Technology Limited, Henoed, Mid-Glamorgan, UK). The column was washed with water (2×50 ml), methanol (2×50 ml) and the product eluted with 2N ammonia in methanol. The fractions containing product were evaporated in vacuo, triuration with iso-hexane/ethyl acetate gave the title compound (0.21 g); NMR Spectrum: (DMSOd6) 0.61 (m, 4H), 2.12 (s, 3H), 2.70 (m, 4H), 2.84 (m, 1H), 3.09 (s, 2H), 3.28 (m, 4H), 7.49 (m, 2H), 7.62 (m, 2H), 7.81 (d, 1H), 7.89 (m, 1H), 8.07 (s, 1H), 8.44 (d, 1H); Mass Spectrum: M+H+ 462.

Provenance & Evidence