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Water → 2-Acetyl-5-(4-fluoro-phenyl)cyclohexane-1,3-dione

HRID 2046465
ノート
印刷プレビュー

反応式

HRID 2046465 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][C:12](=[O:14])[CH2:11][C:10](=[O:15])[CH2:9]2)=[CH:4][CH:3]=1.[C:16]([O-])(=[O:18])[CH3:17].[Na+].C(OCC)(=O)C.O>C(OC(=O)C)(=O)C>[C:16]([CH:11]1[C:12](=[O:14])[CH2:13][CH:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)[CH2:9][C:10]1=[O:15])(=[O:18])[CH3:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 517045Sodium AcetateHCID 7301365-(4-Fluorophenyl)cyclohexane-1,3-dione

生成物 1

HCID 529508832-Acetyl-5-(4-fluoro-phenyl)cyclohexane-1,3-dione

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

反応条件

温度
120 °C

実験手順

5-(4-Fluorophenyl)cyclohexane-1,3-dione (500 mg, 2.4 mmol) and sodium acetate (200 mg, 2.4 mmol) were dissolved in acetic anhydride (5 ml) and heated in a sealed tube at 120° C. for 16 h. The reaction mixture was then allowed to cool to ambient temperature whereupon ethyl acetate (20 ml) and water (10 ml) were added. The organic phase was collected and washed 3 times with a saturated solution of sodium bicarbonate (3×15 ml). The organic phase was dried with MgSO4 and filtered. The solvent was removed under reduced pressure. The title compound was purified by column chromatography using ethyl acetate/heptane (1/3) as the eluent.

後処理

  1. additionwere added
  2. customThe organic phase was collected
  3. washwashed 3 times with a saturated solution of sodium bicarbonate (3×15 ml)
  4. dry with materialThe organic phase was dried with MgSO4
  5. filtrationfiltered
  6. customThe solvent was removed under reduced pressure
  7. customThe title compound was purified by column chromatography

出典と根拠

ORDレコード
ord-43dd97b478c44479b8f357cdcf866fd6
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08592430B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート