Methanol → 1-(Pyridin-4-yl)propan-1-one oxime

HRID 2388193노트

반응식

HRID 2388193 반응식
Cl.[NH2:2][OH:3].C([O-])(=O)C.[Na+].CO.[N:11]1[CH:16]=[CH:15][C:14]([C:17](=O)[CH2:18][CH3:19])=[CH:13][CH:12]=1>CCOC(C)=O.O>[N:11]1[CH:16]=[CH:15][C:14]([C:17](=[N:2][OH:3])[CH2:18][CH3:19])=[CH:13][CH:12]=1

참가 물질

7

반응물 4

HCID 887MethanolHCID 743431-(4-Pyridinyl)-1-propanoneHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium Acetate

생성물 1

HCID 1363417421-(Pyridin-4-yl)propan-1-one oxime수율 95.4%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

Hydroxylamine hydrochloride (2.8 g, 40.7 mmol) and sodium acetate (3.3 g, 40.7 mmol) were added to 20 mL of methanol and the resulting white slurry was stirred at room temperature for 30 min. 1-(Pyridin-4-yl)propan-1-one (5.0 g, 37.0 mmol) was added and the mixture was stirred at room temperature for 20 hours. Water (50 mL) and EtOAc (50 mL) were added and the organic layer was separated. The aqueous layer was basified with solid sodium bicarbonate and extracted with additional EtOAc. The combined organic layer was washed with saturated NaHCO3 solution and dried over MgSO4. The solvent was evaporated in vacuo to give 5.3 g of the title compound. MS: (+) m/z 151.36 (M+1).

후처리

  1. stirringthe mixture was stirred at room temperature for 20 hours
  2. customthe organic layer was separated
  3. extractionextracted with additional EtOAc
  4. washThe combined organic layer was washed with saturated NaHCO3 solution
  5. dry with materialdried over MgSO4
  6. customThe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-0c22f94adf4d4ddcb6804d0d42b32305
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08269008B2

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