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]2

Komponenten

Edukt 2

HCID 24813Phosphorus oxychloride

HCID 178517410HCID 178517410, Verbindung

Produkt 1

HCID 179135596-Bromo-2-chloroquinazoline

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-99daa358aa0e4bb384404a0033d7ade4
Quelldatensatz: uspto-grants-2015_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09126951B2

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