Dimethylformamide → 4-Fluoro-2-nitro-1-propoxybenzene

HRID 1477116노트

반응식

HRID 1477116 반응식
CN(C)C=O.C(=O)([O-])[O-].[K+].[K+].I[CH2:13][CH2:14][CH3:15].[F:16][C:17]1[CH:22]=[CH:21][C:20]([OH:23])=[C:19]([N+:24]([O-:26])=[O:25])[CH:18]=1>O>[F:16][C:17]1[CH:22]=[CH:21][C:20]([O:23][CH2:13][CH2:14][CH3:15])=[C:19]([N+:24]([O-:26])=[O:25])[CH:18]=1

참가 물질

6

반응물 4

HCID 6228Dimethylformamide2회HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 1362364-Fluoro-2-nitrophenol

생성물 1

HCID 669171744-Fluoro-2-nitro-1-propoxybenzene수율 96.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A N,N-dimethylformamide (DMF) solution (3 ml) of potassium carbonate (3.48 g, 25.2 mmol) and 1-iodopropane (3.95 g, 23.2 mmol) was added to a DMF solution (7 ml) of 4-fluoro-2-nitrophenol (3.3 g, 21.0 mmol). The mixture was stirred at room temperature for 48 hours. Water was added to the reaction mixture, and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride solution twice, and concentrated under reduced pressure. The residue was purified using silica gel column chromatography (n-hexane:ethyl acetate=9:1). The purified product was concentrated under reduced pressure to thereby obtain 4.03 g of oily yellow 4-fluoro-2-nitro-1-propoxybenzene (yield: 96%).

후처리

  1. extractionthe resulting mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with a saturated sodium chloride solution twice
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified
  5. concentrationThe purified product was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-04f9775f03d749c2afa0d8fc460d327a
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403773B2

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