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With trichlorophosphate; for 72h;Heating / reflux;
A suspensionof 7-fluoro-2, 4-dioxo(1H, 3X) quinazoline (Method 98,1. 8 g, 10 mmol) inPOC13 (30 ml) was heated under reflux for 72 hours. The brown coloured solution was concentrated to dryness under vacuum. The residue was treated with ice water (50 ml) and filtered. The residue was washed with ice-cold water (10 ml) and dried to give the desired product(1. 7 g, 78%). 1H NMR(CDC13)5 7.92(m,1 H), 7.95 (d, J = 2.9 Hz, 1 H), 8.42(m,1 H). MS: m/z 219 (M+3), 217(M+1).
In ice-water; trichlorophosphate;
b) 164 mg (0.9 mmol) of <strong>[76088-98-7]7-fluoro-1,2,3,4-tetrahydroquinazoline-2,4-dione</strong> were suspended in 3.5 ml (48 mmol) of phosphorus oxychloride and heated to 120 C. for 24 hrs. The reaction mixture was left to cool to room temperature and poured on to ice-water. The brown precipitate was filtered off under suction, dried and chromatographed over silica gel with methylene chloride as the eluent. 130 mg (67%) of 2,4-dichloro-7-fluoroquinazoline were obtained as orange coloured crystals; MS: me/e=216, 218 (M+).
3.82 g
With trichlorophosphate; for 72h;Reflux;
<Step 2> 2,4,-dichloro-7-fluoroquinazoline A mixture of 7-fluoroquinazoline-2,4(1H, 3H)-dione (5.26 g, 29.2 mmol) prepared in Step 1 and phosphorus oxychloride (85 ml) was stirred at reflux for 3 days. After cooling the reaction mixture to room temperature, the same was added into ice water. The resulting solid was filtered and dried in vacuo to give the titled compound (3.82 g) as a yellow solid. 1H NMR (400 MHz, CDCl3) delta 8.32 (m, 1H), 7.63 (d, 1H), 7.49 (t, 1H).
N-(4-(1H-pyrazol-4-yl)phenyl)-2-chloro-7-fluoroquinazolin-4-amine[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
96%
With N-ethyl-N,N-diisopropylamine; In N,N-dimethyl-formamide; at 90.0℃;
A mixture of 4-(lH-pyrazol-4-yl)aniline (120 mg, 0.75 mmol), 2,4-dichloro- 7-fluoroquinazoline (164 mg, 0.75 mmol), and zPrNEt2 (195 mg, 1.51 mmol) in DMF (2.51 mL) was stirred at 90 C overnight, cooled to rt, diluted with water. The precipitate formed was collected by filtration and washed with water and dried in vacuo to provide the title compound (245 mg, 96%). MS (ES+) m/e 340 (M+H)+.
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