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

HRID 1393157

反応式

HRID 1393157 の反応式
[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

参加物

8

反応物 4

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

生成物 1

HCID 765396504-(4-Pyridyl)-2-butanone oxime収率 90%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-461dc5cf49604781892607860c8fd503
出典データセット
uspto-grants-2008_03
特許番号
US07345064B2

関連ノート

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