反応 #684969

ord-eed983d020be4ed8bef379b414531a3b

反応方程式

O
Water
CCOC(C)=O
ethyl acetate
Oc1nccc2ccccc12
1-hydroxyisoquinoline
BrBr
Bromine
Oc1ncc(Br)c2ccccc12
title compound
収率 80.1%
Oc1ncc(Br)c2ccccc12
4-Bromo-1-isoquinolinol
収率 80.1%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the resulting reaction mixture
  2. 2
    ろ過was filtered
  3. 3
    ろ過through filter paper
  4. 4
    洗浄The organic layer was washed with saturated brine
  5. 5
    濃縮concentrated under reduced pressure
  6. 6
    その他The residue was recrystallized from ethyl acetate and hexane

実験手順

Bromine (1.78 ml, 34.5 mmol) was added to an ice-cooled solution of 1-hydroxyisoquinoline (5.01 g, 34.5 mmol) in acetic acid (50 ml), and this reaction mixture was stirred at room temperature for 2 hours. Water, ethyl acetate, and tetrahydrofuran were added, and the resulting reaction mixture was filtered through filter paper. The organic layer was washed with saturated brine and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate and hexane to give the title compound (6.19 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07897387B2uspto-grants-2011_03