Phosphorus oxychloride → 6-Bromo-2-chloro-7-methoxyquinazoline

HRID 524074Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 524074
[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]2

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 178486882HCID 178486882, Verbindung

Produkt 1

HCID 591992766-Bromo-2-chloro-7-methoxyquinazolineAusbeute 75 %

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 h. LCMS showed the reaction was completed. The reaction was cooled to RT, 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

  1. custommost of phosphoryl trichloride was evaporated
  2. additionThe residue was dropwise added to ice water (100 mL)
  3. filtrationthe resulting precipitate was collected via filtration

Quellen und Nachweise

ORD-Eintrag
ord-64f13e311d0d4c8696675b67dc549d23
Quelldatensatz
uspto-grants-2016_05
Patentnummer
US09340514B2

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