Iodoethane → 4-Bromo-5-ethoxy-2-fluoroaniline

HRID 566185노트

반응식

HRID 566185 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](I)[CH3:12].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Br:9][C:5]1[C:6]([O:8][CH2:11][CH3:12])=[CH:7][C:2]([NH2:1])=[C:3]([F:10])[CH:4]=1

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 109656515-Amino-2-bromo-4-fluorophenol

생성물 1

HCID 132814294-Bromo-5-ethoxy-2-fluoroaniline수율 67.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

5-Amino-2-bromo-4-fluorophenol (10.30 g), ethyl iodide (9.36 g) and potassium carbonate (7.59 g) were suspended in acetonitrile (100 ml), and the mixture was heated under refluxing for about 6 hours. After the reaction, the precipitates were filtered, the solvent was distilled off, extracted with ethyl acetate, and 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 v/v) to obtain the objective 4-bromo-5-ethoxy-2-fluoroaniline (7.93 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder refluxing for about 6 hours
  3. customAfter the reaction
  4. filtrationthe precipitates were filtered
  5. distillationthe solvent was distilled off
  6. extractionextracted with ethyl acetate
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThen, ethyl acetate was distilled off
  9. customthe resulting oily substance was purified by chromatography on silica gel (ethyl acetate:n-hexane=1:3 v/v)

출처 및 근거

ORD 기록
ord-a7297898309f4a7787c521b4ba54118e
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06174839B1

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