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

HRID 404718ノート

反応式

HRID 404718 の反応式
[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

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 222501786-Bromoisoquinoline 2-oxide

生成物 1

HCID 222502446-Bromo-1-chloro-isoquinoline

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-27a094df04064df4bb8682d15163dd9a
出典データセット
uspto-grants-2014_06
特許番号
US08748614B2

反応ノート

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