Ethanol → 4,5-Dimethoxyphthalic acid

HRID 2111615

반응식

HRID 2111615 반응식
[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]

참가 물질

5

반응물 4

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

생성물 1

HCID 2909884,5-Dimethoxyphthalic acid

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-49393fb281c54496b9c26fbcfa99448a
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07521451B2

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