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

HRID 18395

반응식

HRID 18395 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, the whole was stirred for 1.5 hours, and then ethyl acetate (50 ml) was added to the reaction mixture to dilute it. Sodium hydrogencarbonate was added thereto. After separation, the organic layer was washed with saturated brine (10 ml), 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 4-(4-pyridyl)-2-butanone oxime (584 mg, 90%) as pale yellow crystals.

후처리

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

출처 및 근거

ORD 기록
ord-a2942a5370974c94897ea627c6c2929b
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741346B2

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