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

HRID 566185ノート

反応式

HRID 566185 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 132814294-Bromo-5-ethoxy-2-fluoroaniline収率 67.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a7297898309f4a7787c521b4ba54118e
出典データセット
uspto-grants-2001_01
特許番号
US06174839B1

反応ノート

読み込み中…