Phosphorus oxychloride → 6-Bromo-2-chloroquinazoline

반응식

[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

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 178517410HCID 178517410, 화합물

생성물 1

HCID 179135596-Bromo-2-chloroquinazoline

실험 절차

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]+.

후처리

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%)

출처 및 근거

ORD 기록: ord-99daa358aa0e4bb384404a0033d7ade4
출처 데이터셋: uspto-grants-2015_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09126951B2

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