Hydroxyamine hydrochloride → 5-Carboxyethyl-2,4-dimethoxy-4'-methoxybenzophenone oxime

HRID 893419노트

반응식

HRID 893419 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([C:11](=O)[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]([OH:25])=[O:24].Cl.[NH2:27][OH:28].C([O-])(=O)C.[Na+]>C(O)C>[C:23]([CH2:22][CH2:21][C:4]1[C:3]([O:2][CH3:1])=[CH:8][C:7]([O:9][CH3:10])=[C:6]([CH:5]=1)[C:11](=[N:27][OH:28])[C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=1)([OH:25])=[O:24]

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 144609963-[2,4-Dimethoxy-5-(4-methoxybenzoyl)phenyl]propionic acid

생성물 1

HCID 867459445-Carboxyethyl-2,4-dimethoxy-4'-methoxybenzophenone oxime

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

37 g of 3-[2,4-dimethoxy-5-(4-methoxybenzoyl)phenyl]propionic acid, 22.4 g of hydroxylamine hydrochloride and 21 g of sodium acetate (anhydrous) are added to 300 ml of absolute ethanol, and the mixture is refluxed with exclusion of moisture for 24 hours. Insolubles are removed by suction, the filtrate is concentrated, and water is added to the residue. The pH is then adjusted to 2 with 1N hydrochloric acid, and the mixture is extracted with ethyl acetate. The organic phase is washed with water, dried over magnesium sulfate and concentrated. The residue is recrystallized from ethyl acetate/hexane.

후처리

  1. temperaturethe mixture is refluxed with exclusion of moisture for 24 hours
  2. customInsolubles are removed by suction
  3. concentrationthe filtrate is concentrated
  4. additionwater is added to the residue
  5. extractionthe mixture is extracted with ethyl acetate
  6. washThe organic phase is washed with water
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated
  9. customThe residue is recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-0237181bebd849ebaf988bb108ec4ff4
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05124478

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