Sodium Carbonate → 4-(4-Pyridyl)-2-butanone oxime

HRID 11453

반응식

HRID 11453 반응식
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][CH2:8][C:9](=O)[CH3:10])=[CH:3][CH:2]=1.C(=O)([O-])[O-].[Na+].[Na+].Cl.[NH2:19][OH:20].C(=O)([O-])O.[Na+]>C(OCC)(=O)C.O1CCCC1.O>[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][CH2:8][C:9](=[N:19][OH:20])[CH3:10])=[CH:3][CH:2]=1

참가 물질

8

반응물 4

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 127072234-(Pyridin-4-yl)butan-2-one

생성물 1

HCID 765396504-(4-Pyridyl)-2-butanone oxime수율 90%

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

Next, water (12 ml) and tetrahydrofuran (1.2 ml) were added to 4-(4-pyridyl)-2-butanone (736 mg, 3.96 mmol), and the mixture was stirred at room temperature. Sodium carbonate (483 mg, 4.56 mmol) and hydroxylamine hydrochloride (358 mg, 5.15 mmol) were added to the mixture, and the whole was stirred for 1.5 hours and then diluted with ethyl acetate (50 ml). Sodium hydrogencarbonate was added thereto, layers were separated, and the organic layer was washed with saturated brine (10 ml). The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. Cyclohexane was added to the resulting crystals, and the crystals were filtered off to give 584 mg (90%) of 4-(4-pyridyl)-2-butanoneoxime as pale yellow crystals.

후처리

  1. stirringthe whole was stirred for 1.5 hours
  2. customlayers were separated
  3. washthe organic layer was washed with saturated brine (10 ml)
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionCyclohexane was added to the resulting crystals
  7. filtrationthe crystals were filtered off

출처 및 근거

ORD 기록
ord-0bf8c05fbae940ba8dcec8a3c39101cf
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098226B2

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