2,4-DICHLORO-6,7-DIFLUOROQUINAZOLINE synthesis
- Product Name:2,4-DICHLORO-6,7-DIFLUOROQUINAZOLINE
- CAS Number:774212-69-0
- Molecular formula:C8H2Cl2F2N2
- Molecular Weight:235.02
769158-54-5
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774212-69-0
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Yield:774212-69-0 88%
Reaction Conditions:
with N,N-dimethyl-aniline;trichlorophosphate at 120; for 7 h;Heating / reflux;
Steps:
890.B Step B : Synthesis of 2,4-dichloro-6,7-difluoroquinazoline
To a suspension of 6,7-difluoro-1H-quinazoline-2,4-dione (6.9 g, 35 mmol) in POCl3 (21 mL) , VA ; CLOWLY added N,N-dimethylaniline (4.9 mL, 35 mmol). The reaction was heated at reflux (120 °C) FOR 7 H UNTIL the starting material was completely dissolved and the entire solution N D D RK purple color. The reaction was allowed to cool and poured very slowly onto ice (1 L); watch out for heat generation . . The resulting precipitate was filtered and washed with ice water. The crude product was purified from a short column of silica with CH2Cl2 as an eluting solvent. The desired product (7, 2 S8 %) was obtained as a white solid. ESI MS M/E 236 M+H+; 1H NMR (400 MHZ, CDCL3) No. 8.01 (DD, J=9.2, 8.0 HZ, 1 H), 7.76 (DD, J=10.0 7.2 Hz, 1 H).
References:
WO2004/87680,2004,A1 Location in patent:Page 166-167
83506-93-8
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774212-69-0
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207346-42-7
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774212-69-0
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