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

HRID 18395

反応式

HRID 18395 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, 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.

後処理

  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

出典と根拠

ORDレコード
ord-a2942a5370974c94897ea627c6c2929b
出典データセット
uspto-grants-2010_06
特許番号
US07741346B2

関連ノート

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