Phosphorus oxychloride → 6-Bromo-2-chloroquinazoline

反応式

[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

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 178517410HCID 178517410、化合物

生成物 1

HCID 179135596-Bromo-2-chloroquinazoline収率 87%

実験手順

A solution of 6-bromoquinazolin-2-ol (9.72 g, 40 mmol) in phosphorus oxychloride (100 mL) was refluxed for 5 hours. The reaction was cooled to room temperature, 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]+.

後処理

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

出典と根拠

ORDレコード: ord-4034d431f2ba45729290c605eed1477d
出典データセット: uspto-grants-2016_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09434700B2

反応ノート

読み込み中…

参加物