7-Bromo-1-Chloroisoquinoline → 7-Bromoisoquinoline

HRID 14253

反応式

HRID 14253 の反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8]=[C:9]2Cl)=[CH:4][CH:3]=1>C(O)(=O)C.[Zn]>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8]=[CH:9]2)=[CH:4][CH:3]=1

参加物

4

反応物 1

HCID 65020247-Bromo-1-Chloroisoquinoline

生成物 1

HCID 122574417-Bromoisoquinoline収率 86.8%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

実験手順

A solution of 7-bromo-1-chloroisoquinoline (2.50 g, 10.3 mmol) and activated zinc (1.40 g, 21.65 mmol) in acetic acid (20 mL) was heated at reflux for 2 h. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. The resulting residue was partitioned between ethyl acetate and water. The organic layer was washed with saturated sodium chloride, dried (sodium sulfate), filtered, and concentrated under reduced pressure to provide 7-bromoisoquinoline (1.86 g): ESI MS m/z 208 [M+H]+.

後処理

  1. temperatureat reflux for 2 h
  2. concentrationconcentrated under reduced pressure
  3. customThe resulting residue was partitioned between ethyl acetate and water
  4. washThe organic layer was washed with saturated sodium chloride
  5. dry with materialdried (sodium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-51725a07dc75426cb2d226d4e7ea7d78
出典データセット
uspto-grants-2010_06
特許番号
US07727997B2

関連ノート

読み込み中…