Sodium Hydroxide → 3-[2,4-Dimethoxy-5-(4-methoxybenzoyl)phenyl]propionic acid

HRID 893418노트

반응식

HRID 893418 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([C:11](=[O:20])[C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)=[CH:5][C:4]=1[CH2:21][CH2:22][C:23]([O:25]C)=[O:24].[OH-].[Na+]>O1CCOCC1>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([C:11](=[O:20])[C:12]2[CH:13]=[CH:14][C:15]([O:18][CH3:19])=[CH:16][CH:17]=2)=[CH:5][C:4]=1[CH2:21][CH2:22][C:23]([OH:25])=[O:24]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 14460995Methyl 3-[2,4-dimethoxy-5-(4-methoxybenzoyl)phenyl]propionate

생성물 1

HCID 144609963-[2,4-Dimethoxy-5-(4-methoxybenzoyl)phenyl]propionic acid

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

60.9 g of methyl 3-[2,4-dimethoxy-5-(4-methoxybenzoyl)phenyl]propionate are mixed with 300 ml of 2N sodium hydroxide solution and 300 ml of dioxane and stirred overnight. The dioxane is then removed in vacuo, and the alkaline aqueous solution is extracted once with 100 ml of ethyl acetate. The aqueous phase is adjusted to pH 2 with concentrated hydrochloric acid, when part of the product separates out. The mixture is extracted three times with 200 ml of ethyl acetate each time, and the organic phase is washed with water, dried over sodium sulfate and concentrated. The residue is recrystallized from ethyl acetate/acetone/hexane.

후처리

  1. customThe dioxane is then removed in vacuo
  2. extractionthe alkaline aqueous solution is extracted once with 100 ml of ethyl acetate
  3. extractionThe mixture is extracted three times with 200 ml of ethyl acetate each time
  4. washthe organic phase is washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue is recrystallized from ethyl acetate/acetone/hexane

출처 및 근거

ORD 기록
ord-c243e0a9001f4ea59539d42c52d1062f
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05124478

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