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

HRID 2167449ノート

反応式

HRID 2167449 の反応式
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

参加物

6

反応物 4

HCID 6228Dimethylformamide2 回HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 1362364-Fluoro-2-nitrophenol

生成物 1

HCID 669171744-Fluoro-2-nitro-1-propoxybenzene収率 96.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-8c8eff71e053467e8b3cf949e5d42629
出典データセット
uspto-grants-2015_06
特許番号
US09045464B2

反応ノート

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