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2,4,7-trichloro-6-fluoro-quinazoline synthesis

2synthesis methods
2,4(1H,3H)-Quinazolinedione, 7-chloro-6-fluoro-

174565-49-2
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2,4,7-trichloro-6-fluoro-quinazoline

174566-16-6
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Yield:174566-16-6 1.45 g (82%)

Reaction Conditions:

in ice-water;trichlorophosphate;

Steps:

10.b 8-Chloro-9-fluoro-2,3,5,6-tetrahydro-1,2,4-triazolo[4,3-c]quinazoline-3,5-dione

b) 1.5 g (0.0070 mol) of 7-chloro-6-fluoro-1,2,3,4-tetrahydroquinazoline-2,4-dione were suspended in 9.6 ml (0.10 mol) of phosphorus oxychloride and heated to 105° C. for 84 hrs. The reaction mixture was left to cool to room temperature and poured on to ice-water. The brown precipitate was extracted with dichloromethane and chromatographed over silica gel with dichloromethane as the eluent. Yield: 1.45 g (82%) of 2,4,7-trichloro-6-fluoro-quinazoline as yellowish crystals; m.p. 90°-92° C.

References:

US5688803,1997,A