反应详情

{4-[(3-Chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methanol (0.20 g, 0.604 mmol) was added to neat thionyl chloride (1 ml) over a period of 5 minutes. The resulting solution was stirred for 30 minutes, concentrated to dryness and the residue was subjected to an azeotropic distillation with toluene (2×10 ml). The resulting solid was triturated with acetonitrile (5 ml) filtered and dried to a constant weight in a vacuum oven at 40° C. to give the hydrochloride salt of N-(3-chloro-2-fluorophenyl)-6-(chloromethyl)-7-methoxyquinazolin-4-amine (0.21 g, 100%) as a white solid; Mass Spectrum: (M+H)+ 352.

1. concentrationconcentrated to dryness
2. distillationthe residue was subjected to an azeotropic distillation with toluene (2×10 ml)
3. customThe resulting solid was triturated with acetonitrile (5 ml)
4. filtrationfiltered
5. customdried to a constant weight in a vacuum oven at 40° C.