Potassium Carbonate → Ethyl 2-(2-acetyl-4-fluorophenoxy)acetate

HRID 1582754ノート

反応式

HRID 1582754 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1.I[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:17]([O:16][C:14](=[O:15])[CH2:13][O:11][C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:7][C:6]=1[C:8](=[O:10])[CH3:9])[CH3:18]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12183Ethyl iodoacetateHCID 959922-Acetyl-4-fluorophenol

生成物 1

HCID 22718336Ethyl 2-(2-acetyl-4-fluorophenoxy)acetate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

5′-Fluoro-2′-hydroxyacetophenone 2.0 g, ethyl iodoacetate 4.16 g and potassium carbonate 2.7 g were added to acetone 43 ml in a nitrogen atmosphere, and the mixture was stirred overnight under reflux with heating. After cooled to room temperature, the potassium carbonate was filtered off through Celite, and the filtrate was partitioned by adding water and ethyl acetate. The organic layer was washed with water and then with brine, dried over magnesium sulfate anhydride, and evaporated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate system), whereby the title compound 3.07 g, 99% was obtained as a colorless oil.

後処理

  1. temperatureunder reflux
  2. temperaturewith heating
  3. filtrationthe potassium carbonate was filtered off through Celite
  4. customthe filtrate was partitioned
  5. additionby adding water and ethyl acetate
  6. washThe organic layer was washed with water
  7. dry with materialwith brine, dried over magnesium sulfate anhydride
  8. customevaporated
  9. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate system), whereby the title compound 3.07 g, 99%
  10. customwas obtained as a colorless oil

出典と根拠

ORDレコード
ord-dacc81cb9c9342508ac19aab38d403d4
出典データセット
uspto-grants-2004_05
特許番号
US06737425B1

反応ノート

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