Phosphorus oxychloride → 6-Bromo-1-chloro-isoquinoline

HRID 404718노트

반응식

HRID 404718 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[N+:7]([O-])[CH: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)[C:8]([Cl:15])=[N:7][CH:6]=[CH:5]2

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 222501786-Bromoisoquinoline 2-oxide

생성물 1

HCID 222502446-Bromo-1-chloro-isoquinoline

실험 절차

53.0 g (236, mmol) of 6-bromo-isoquinoline 2-oxide (4) were heated in 400 ml of POCl3 under reflux conditions in two portions. After 4 h, the reaction was cooled to room temperature and poured carefully on ice with mechanical stirring. The aqueous solution was extracted three times with dichloromethane. The combined organic layers were dried over magnesium sulfate and evaporated, which gave 42.8 g of the title compound, which was used without further purification. Rt=1.64 min (Method C). Detected mass: 242.1/244.2 (M+H+).

후처리

  1. additionpoured carefully on ice with mechanical stirring
  2. extractionThe aqueous solution was extracted three times with dichloromethane
  3. dry with materialThe combined organic layers were dried over magnesium sulfate
  4. customevaporated

출처 및 근거

ORD 기록
ord-27a094df04064df4bb8682d15163dd9a
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748614B2

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