thionyl chloride; trichlorophosphate; n,n-dimethyl-formamide
reactants are commercially availlable.
hanmi pharm. co., ltd., wo2007/55514, a1, (2007) < 1 -4> 4-chloro-7-fluoro-6-nitro-quinazoline; the compound of (20 g, 96 mmol), thionyl chloride (170 ml), phosphorousoxy chloride (30 ml) and n,n-dimethylformamide (1 ml) were added into a reaction bottle and stirred. the resulting solution was heated to 100°c until the mixture was melted transparently, and then stirred for 2 hours. the reaction temperature was cooled to room temperature, and the solution was distilled under a reduced pressure to remove the solvent. the resulting residue was distilled again after adding 300 ml of toluene thereto, and the procedure was repeated three times to obtain the title compound 21 g (yield: 99percent).1h nmr (cdcl3) delta: 7.73 (d, ih), 8.30 (s, ih)5 8.7 2 (d, ih).
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