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

HRID 573973노트

반응식

HRID 573973 반응식
[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

참가 물질

4

반응물 2

HCID 24408BromineHCID 218230207-Fluoroquinolin-8-ol

생성물 1

HCID 443611965-Bromo-7-fluoro-8-quinolinol수율 101.6%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c7d3b8f85f9f4d37977c01f0258e0cd0
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034303B2

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