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

HRID 358884노트

반응식

HRID 358884 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 27827542,3-Difluoro-6-nitroanisole수율 106.7%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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)].

후처리

  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

출처 및 근거

ORD 기록
ord-3edc267b0f534fc48314e44229357d05
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997943

반응 노트

불러오는 중…