Potassium Carbonate → 1-Benzyl-3-(hydroxyimino)-4-methylpyrrolidine

HRID 358908Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 358908
[CH2:1]([N:8]1[CH2:12][CH:11]([CH3:13])[C:10](=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:16][OH:17].C(=O)([O-])[O-].[K+].[K+]>C(O)C.O>[CH2:1]([N:8]1[CH2:12][CH:11]([CH3:13])[C:10](=[N:16][OH:17])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 124309801-Benzyl-4-methylpyrrolidin-3-one

Produkt 1

HCID 859932571-Benzyl-3-(hydroxyimino)-4-methylpyrrolidineAusbeute 107,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

A solution of 31.7 g (0.168 mole) of 1-benzyl-4-methyl-3-pyrrolidone [prepared as described in Step (4) above] dissolved in 200 ml of ethanol was added dropwise to a solution of 59.4 g (0.79 mole) of hydroxylamine hydrochloride dissolved in 200 ml of water over a period of 1 hour, whilst keeping the temperature at 20° to 25° C. 62.1 g (0.45 mole) of potassium carbonate were then added, and the mixture was stirred at room temperature overnight, after which it was diluted with 100 ml of water. The aqueous solution was extracted with chloroform, and the chloroform extract was washed with water, dried and concentrated by evaporation under reduced pressure, to give 36.9 g of 1-benzyl-3-(hydroxyimino)-4-methylpyrrolidine as brown crystals.

Aufarbeitung

  1. customat 20° to 25° C
  2. extractionThe aqueous solution was extracted with chloroform
  3. extractionthe chloroform extract
  4. washwas washed with water
  5. customdried
  6. concentrationconcentrated by evaporation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-fac065dec23f4efab27fae3f72637d10
Quelldatensatz
uspto-grants-1991_03
Patentnummer
US04997943

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