反应详情

A solution of concentrated hydrochloric acid (5 ml) in 1,4-dioxan (25 ml) was added dropwise to a solution of tert-butyl 3-(aminocarbonyl)-3-[({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)(methyl)amino]azetidine-1-carboxylate (303 mg, 0.56 mmol) in 1,4-dioxan (6 ml). The reaction mixture was stirred overnight, then concentrated under reduced pressure. The residues were triturated with a mixture of methanol/dichloromethane/diethylether to give the hydrochloride salt of 3-[({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)(methyl)amino]azetidine-3-carboxamide as a solid (330 mg, 100%); 1H NMR Spectrum: (DMSO-d6) 2.19 (s, 3H), 3.73 (s, 2H), 3.95 (brd, 2H), 4.04 (s, 3H), 4.13 (brd, 2H), 7.38 (m, 2H), 7.56 (t, 1H), 7.61 (s, 1H), 7.66 (s, 1H), 7.75 (brs, 1H), 8.92 (s, 1H), 8.92 (brs, 1H), 9.30 (s, 1H), 9.80 (brs, 1H); Mass Spectrum: (M+H)+ 445.

1. concentrationconcentrated under reduced pressure
2. customThe residues were triturated with a mixture of methanol/dichloromethane/diethylether