Phosphorus oxychloride → 6-Bromo-2-chloroquinazoline
Reaktionsgleichung
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7](O)[N:6]=[CH:5]2.O=P(Cl)(Cl)[Cl:15]>>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([Cl:15])[N:6]=[CH:5]2Komponenten
3
Versuchsvorschrift
A solution of 6-bromoquinazolin-2-ol (31) (6.0 g, 26.7 mmol) in POCl3 (80 mL) was refluxed at 110° C. for 5 hours. An aliquot of the reaction mixture was analyzed by LCMS and indicated that the reaction had proceeded to completion. Most of POCl3 was removed under reduced pressure, and the residue was added dropwise to ice water (500 mL). The resulting precipitate was collected via filtration as a yellow solid (3.5 g, 54%). MS (ES+) C8H4BrClN2 requires: 242. found: 243, 245 [M+H]+.
Aufarbeitung
- customMost of POCl3 was removed under reduced pressure
- additionthe residue was added dropwise to ice water (500 mL)
- filtrationThe resulting precipitate was collected via filtration as a yellow solid (3.5 g, 54%)
Quellen und Nachweise
- ORD-Eintrag
- ord-25992e7f8ead4927aa58d8dd9cb79fc0
- Quelldatensatz
- uspto-grants-2016_05
- Patentnummer
- US09340514B2
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