Potassium Hydroxide → 4-Fluoro-2,3-dimethoxybenzene butanoic acid

HRID 979806ノート

反応式

HRID 979806 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][CH:11]=[O:12])=[C:4]([O:13][CH3:14])[C:3]=1[O:15][CH3:16].[OH-:17].[K+]>O.C(O)C.[Ag]=O.[N+]([O-])([O-])=O.[Ag+]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][C:11]([OH:17])=[O:12])=[C:4]([O:13][CH3:14])[C:3]=1[O:15][CH3:16]

参加物

7

反応物 2

HCID 14797Potassium HydroxideHCID 571383154-Fluoro-2,3-dimethoxybenzene butanal

生成物 1

HCID 867411834-Fluoro-2,3-dimethoxybenzene butanoic acid収率 30%

試薬・触媒・溶媒 4

HCID 24470Silver Nitrate触媒HCID 92152Silver(II) oxide触媒HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

The product from Example 55 (12.6 g) was oxidized with silver oxide prepared in situ from a solution of silver nitrate (15.6 g) in H2O (22 ml) and potassium hydroxide (12.7 g) in H2O (22 ml). The reaction was done in ethanol (170 ml) with stirring at room temperature. After 1 hour, the precipitated silver salts were filtered, washed with water and concentrated to 1/2 volume. The aqueous basic layer was diluted with water extracted with hexane several times, acidified and extracted with ethyl acetate. The organic layer was separated, dried and evaporated to afford the desired acid in 30% yield.

後処理

  1. filtrationthe precipitated silver salts were filtered
  2. washwashed with water
  3. concentrationconcentrated to 1/2 volume
  4. additionThe aqueous basic layer was diluted with water
  5. extractionextracted with hexane several times
  6. extractionextracted with ethyl acetate
  7. customThe organic layer was separated
  8. customdried
  9. customevaporated

出典と根拠

ORDレコード
ord-7a71f5c47a55487b85dc01e91df675b1
出典データセット
uspto-grants-1987_01
特許番号
US04634705

反応ノート

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