Phosphorus oxychloride → 6-Bromo-2-chloro-7-methoxyquinazoline
Reaktionsgleichung
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[N:8]=[C:7](O)[N:6]=[CH:5]2.P(Cl)(Cl)([Cl:17])=O>>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[N:8]=[C:7]([Cl:17])[N:6]=[CH:5]2Komponenten
3
Versuchsvorschrift
To a solution of 6-bromo-7-methoxyquinazolin-2-ol (3.0 g, 11.8 mmol) in phosphoryl trichloride (30 mL) was refluxed at 130° C. for 5 hours. The reaction was cooled to room temperature, and most of phosphoryl trichloride was evaporated. The residue was dropwise added to ice water (100 mL), and the resulting precipitate was collected via filtration to give the title compound as a yellow solid (2.4 g, 75%). MS (ES+) C9H6BrClN2O requires: 272, 274, found: 273, 275 [M+H]+.
Aufarbeitung
- custommost of phosphoryl trichloride was evaporated
- additionThe residue was dropwise added to ice water (100 mL)
- filtrationthe resulting precipitate was collected via filtration
Quellen und Nachweise
- ORD-Eintrag
- ord-54f87fe5431647338e937c62ae14b6cb
- Quelldatensatz
- uspto-grants-2016_09
- Patentnummer
- US09434700B2
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