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

HRID 979806노트

반응식

HRID 979806 반응식
[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]

참가 물질

7

반응물 2

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

생성물 1

HCID 867411834-Fluoro-2,3-dimethoxybenzene butanoic acid수율 30%

시약·촉매·용매 4

HCID 24470Silver Nitrate촉매HCID 92152Silver(II) oxide촉매HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7a71f5c47a55487b85dc01e91df675b1
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04634705

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