Hydrazine hydrate (1:1) → HCID 178423887, Verbindung

HRID 721984

Reaktionsgleichung

Reaktionsgleichung von HRID 721984
C[N:2]([CH:4]=[C:5]1[CH2:9][CH2:8][C:7]([CH3:11])([CH3:10])[C:6]1=O)C.O.[NH2:14]N>C(O)C>[CH3:10][C:7]1([CH3:11])[C:6]2[C:5](=[CH:4][NH:2][N:14]=2)[CH2:9][CH2:8]1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 695835902-[(Dimethylamino)methylene]-5,5-dimethylcyclopentanone

Produkt 1

HCID 178423887HCID 178423887, VerbindungAusbeute 102,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of 2-[(dimethylamino)methylene]-5,5-dimethylcyclopentanone (12.5 g, 75 mmol) in ethanol (100 mL) at room temperature was added hydrazine hydrate (4 mL, 82.3 mmol). The reaction mixture was heated at reflux overnight. It was then cooled to room temperature and concentrated. Water (700 mL) was added to the residue, and the resulting solution was extracted twice with diethyl ether (2×250 mL). The organic extracts were combined, dried over MgSO4 and concentrated to give the title compound as an oil (10.5 g). 1H NMR indicated the oil to be ˜60% pure. It was used directly for Step C.

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux overnight
  3. concentrationconcentrated
  4. additionWater (700 mL) was added to the residue
  5. extractionthe resulting solution was extracted twice with diethyl ether (2×250 mL)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-f657392d3ec74be3a5f9a13e2dda1db6
Quelldatensatz
uspto-grants-2006_11
Patentnummer
US07138361B2

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