Methyl iodide → 2,3-Difluoroanisole

HRID 897140

반응식

HRID 897140 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:9].[C:10]([O-])([O-])=O.[K+].[K+].IC>CN(C=O)C>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[O:9][CH3:10]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 808792,3-Difluorophenol

생성물 1

HCID 27693442,3-Difluoroanisole수율 75.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2,3-Difluorophenol (4.55 g) was dissolved in DMF (25 mL) and was treated with powdered K2CO3 (6.0 grams) and the mixture was stirred at an ambient temperature for 10 minutes under nitrogen atmosphere. The mixture was treated with iodomethane (9.0 grams), and was stirred at room temperature for 18 hours. The reaction mixture was quenched with water and was extracted with ether. The ether extract was washed with water, dried (Na2SO4) and concentrated to afford 3.8 grams of title compound as amber oil. 1HNMR(CDCl3): δ 6.97(m, 1H), 6.78(m, 2H), 3.90(s, 3H). Step 2: 2,3-Difluoro-4-methoxybenzaldehyde.

후처리

  1. stirringwas stirred at room temperature for 18 hours
  2. customThe reaction mixture was quenched with water
  3. extractionwas extracted with ether
  4. extractionThe ether extract
  5. washwas washed with water
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f1b8da9c2eb14fada23a8be65ec8822b
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06921767B2

연결된 노트

불러오는 중…