Methyl iodide → 2,3-Difluoro-6-nitroanisole

HRID 358884ノート

反応式

HRID 358884 の反応式
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([N+:9]([O-:11])=[O:10])[C:3]=1[OH:12].[C:13](=O)([O-])[O-].[K+].[K+].CI>CC(C)=O>[F:1][C:2]1[C:3]([O:12][CH3:13])=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27337452,3-Difluoro-6-nitrophenol

生成物 1

HCID 27827542,3-Difluoro-6-nitroanisole収率 106.7%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

20 g (0.114 mole) of 2,3-difluoro-6-nitrophenol (VI) were dissolved in 700 ml of acetone. 18.9 g (0.137 mole) of potassium carbonate and 34.1 g (0.24 mole) of methyl iodide were added to the solution, and the mixture was heated under reflux for 20 hours, whilst stirring. The solvent was then removed from the mixture by evaporation under reduced pressure, and the residue was extracted with ethyl acetate. The ethyl acetate extract was washed with water and dried, and the solvent was removed by evaporation under reduced pressure to give 23.0 g of 3,4-difluoro-2-methoxy-1-nitrobenzene (VII) as a yellow oil [Step (B1)].

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 20 hours
  3. customThe solvent was then removed from the mixture by evaporation under reduced pressure
  4. extractionthe residue was extracted with ethyl acetate
  5. extractionThe ethyl acetate extract
  6. washwas washed with water
  7. customdried
  8. customthe solvent was removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-3edc267b0f534fc48314e44229357d05
出典データセット
uspto-grants-1991_03
特許番号
US04997943

反応ノート

読み込み中…