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.P(Cl)(Cl)([Cl:15])=O>>[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]2

Komponenten

Edukt 2

HCID 24813Phosphorus oxychloride

HCID 178517410HCID 178517410, Verbindung

Produkt 1

HCID 179135596-Bromo-2-chloroquinazolineAusbeute 87 %

Versuchsvorschrift

A solution of 6-bromoquinazolin-2-ol (9.72 g, 40 mmol) in phosphorus oxychloride (100 mL) was refluxed for 5 h. LCMS showed the reaction was completed. The reaction was cooled to RT, and most of phosphorus oxychloride was removed under reduced pressure. The residue was dropwise added to ice water (500 mL), and the resulting precipitate was collected by the filtration to give the title compound (9 g, 87%) as a yellow solid. MS (ES+) C8H3BrClFN2 requires: 260, 262. Found: 261, 263 [M+H]+.

Aufarbeitung

custommost of phosphorus oxychloride was removed under reduced pressure
additionThe residue was dropwise added to ice water (500 mL)
filtrationthe resulting precipitate was collected by the filtration

Quellen und Nachweise

ORD-Eintrag: ord-ea6748a923694cffb537e8e07c69f441
Quelldatensatz: uspto-grants-2015_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09126951B2

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