Allyl bromide → 5-Allyloxy-4-bromo-2-fluoroaniline

HRID 566195노트

반응식

HRID 566195 반응식
[NH2:1][C:2]1[C:3]([F:10])=[CH:4][C:5]([Br:9])=[C:6]([OH:8])[CH:7]=1.[CH2:11](Br)[CH:12]=[CH2:13].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:13]([O:8][C:6]1[C:5]([Br:9])=[CH:4][C:3]([F:10])=[C:2]([CH:7]=1)[NH2:1])[CH:12]=[CH2:11]

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 109656515-Amino-2-bromo-4-fluorophenol

생성물 1

HCID 212655985-Allyloxy-4-bromo-2-fluoroaniline수율 32.9%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

5-Amino-2-bromo-4-fluorophenol (30.9 g), allyl bromide (21.8 g) and potassium carbonate (22.77 g) were suspended in acetonitrile (300 ml), and the mixture was stirred at room temperature for 12 hours. After the reaction, the precipitates were filtered, the solvent was distilled off, and this was extracted with ethyl acetate. After washing with water, it was dried over anhydrous magnesium sulfate. Then, ethyl acetate was distilled off and the resulting oily substance was purified by chromatography on silica gel (ethyl acetate:n-hexane=1:3) to obtain the objective 5-allyloxy-4-bromo-2-fluoroaniline (12.14 g).

후처리

  1. customAfter the reaction
  2. filtrationthe precipitates were filtered
  3. distillationthe solvent was distilled off
  4. extractionthis was extracted with ethyl acetate
  5. washAfter washing with water, it
  6. dry with materialwas dried over anhydrous magnesium sulfate
  7. distillationThen, ethyl acetate was distilled off
  8. customthe resulting oily substance was purified by chromatography on silica gel (ethyl acetate:n-hexane=1:3)

출처 및 근거

ORD 기록
ord-b3d8c62272b443e0bc028e62b5887f53
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06174839B1

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