Dimethylformamide → 4-(2-Fluorophenoxy)benzaldehyde

HRID 640323

反応式

HRID 640323 の反応式
CN(C)C=O.[F:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[OH:13].F[C:15]1[CH:22]=[CH:21][C:18]([CH:19]=[O:20])=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+]>O>[F:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[O:13][C:15]1[CH:22]=[CH:21][C:18]([CH:19]=[O:20])=[CH:17][CH:16]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 97072-FluorophenolHCID 11430Potassium CarbonateHCID 680234-Fluorobenzaldehyde

生成物 1

HCID 107987454-(2-Fluorophenoxy)benzaldehyde収率 99.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To an N,N-dimethylformamide (30.0 mL) solution of 2-fluorophenol (5.43 g, 48.4 mmol) and 4-fluorobenzaldehyde (3.00 g, 24.2 mmol) was added potassium carbonate (10.1 g, 72.5 mmol) under nitrogen atmosphere, which was stirred for 16 hours at 80° C. Water was added to the reaction solution at room temperature, which was then extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:15→1:10) to obtain the title compound (5.20 g, 99.4%).

後処理

  1. extractionwhich was then extracted with ethyl acetate
  2. washThe organic layer was washed with saturated aqueous sodium chloride
  3. customthe solvent was evaporated under a reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:15→1:10)

出典と根拠

ORDレコード
ord-d199810d531549f097cd3bc22be7c567
出典データセット
uspto-grants-2010_04
特許番号
US07691882B2

関連ノート

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