Ethanol → 4,5-Dimethoxyphthalic acid

HRID 2111615

反応式

HRID 2111615 の反応式
[OH-:1].[Na+].[CH3:3][O:4][C:5]1[C:14]([O:15][CH3:16])=[CH:13][CH:12]=[C:11]2[C:6]=1C[O:8][C:9]2=[O:10].[Mn]([O-])(=O)(=O)=O.[K+].[CH2:23]([OH:25])C>>[CH3:16][O:15][C:14]1[CH:13]=[C:12]([C:23]([OH:25])=[O:1])[C:11](=[CH:6][C:5]=1[O:4][CH3:3])[C:9]([OH:8])=[O:10]

参加物

5

反応物 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 516875Potassium PermanganateHCID 126376234,5-Dimethoxy-2-benzofuran-1(3H)-one

生成物 1

HCID 2909884,5-Dimethoxyphthalic acid

反応条件

温度
25 °C

実験手順

An aqueous 2N sodium hydroxide solution of the product of above-mentioned (a) (3.0 g, 15 mmol) was added dropwise with stirring to a 6% aqueous solution of potassium permanganate (50 ml) under ice cooling, and the reaction solution was stirred overnight with gradually raising the temperature to 25° C. To the reaction solution was added ethanol and the precipitated manganese dioxide was filtered off. The filtrate was acidified with concentrated hydrochloric acid and concentrated under reduced pressure. To the residue was added methanol and stirred for 10 minutes. After the insoluble materials were filtered off, the filtrate was concentrated under reduced pressure to give 4.1 g of 4,5-dimethoxyphthalic acid.

後処理

  1. filtrationthe precipitated manganese dioxide was filtered off
  2. concentrationconcentrated under reduced pressure
  3. additionTo the residue was added methanol
  4. stirringstirred for 10 minutes
  5. filtrationAfter the insoluble materials were filtered off
  6. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-49393fb281c54496b9c26fbcfa99448a
出典データセット
uspto-grants-2009_04
特許番号
US07521451B2

関連ノート

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