反应详情

Trifluoroacetic acid (1 ml) was added to a stirred solution of tert-butyl 4-(aminocarbonyl)-4-[({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)(methyl)amino]piperidine-1-carboxylate (0.35 g, 0.612 mmol) in dichloromethane (1 ml) at room temperature. The resulting solution was stirred for 1 hour, concentrated to dryness and the residue re-dissolved in dichloromethane (1 ml). 4.0 M hydrogen chloride in dioxane (1 ml) was then added to give a white precipitate. This was collected by filtration, washed with diethyl ether (2×10 ml) and dried to a constant weight to give 4-[({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)(methyl)amino]piperidine-4-carboxamide hydrochloride (0.35 g, 100%), as a white solid; Mass Spectrum: (M+H)+ 473.

1. concentrationconcentrated to dryness
2. dissolutionthe residue re-dissolved in dichloromethane (1 ml)
3. addition4.0 M hydrogen chloride in dioxane (1 ml) was then added
4. customto give a white precipitate
5. filtrationThis was collected by filtration
6. washwashed with diethyl ether (2×10 ml)
7. customdried to a constant weight