Bromine → 5-Bromo-7-fluoro-8-quinolinol

HRID 573973ノート

反応式

HRID 573973 の反応式
[Br:1]Br.[F:3][C:4]1[C:13]([OH:14])=[C:12]2[C:7]([CH:8]=[CH:9][CH:10]=[N:11]2)=[CH:6][CH:5]=1>C(O)(=O)C>[Br:1][C:6]1[CH:5]=[C:4]([F:3])[C:13]([OH:14])=[C:12]2[C:7]=1[CH:8]=[CH:9][CH:10]=[N:11]2

参加物

4

反応物 2

HCID 24408BromineHCID 218230207-Fluoroquinolin-8-ol

生成物 1

HCID 443611965-Bromo-7-fluoro-8-quinolinol収率 101.6%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

An rt solution of bromine (2.34 g, 14.7 mmol) in acetic acid (10 mL) was slowly added to a solution of 7-fluoro-8-quinolinol (2.0 g, 12.2 mmol) in acetic acid (30 mL). The brown reaction mixture was stirred at rt for 16 h, after which the mixture was quenched with saturated sodium bisulfite solution. The resulting mixture was extracted with methyl t-butyl ether 3 times. The combined organic phases were washed with saturated NaHCO3 and brine, dried over Na2SO4, and concentrated in vacuo to dryness to give 3.0 g (97.0%) 5-bromo-7-fluoro-8-quinolinol as a green solid.

後処理

  1. customafter which the mixture was quenched with saturated sodium bisulfite solution
  2. extractionThe resulting mixture was extracted with methyl t-butyl ether 3 times
  3. washThe combined organic phases were washed with saturated NaHCO3 and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo to dryness

出典と根拠

ORDレコード
ord-c7d3b8f85f9f4d37977c01f0258e0cd0
出典データセット
uspto-grants-2015_05
特許番号
US09034303B2

反応ノート

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