1,2-Diethylhydrazine dihydrochloride → HCID 10442180, Verbindung

HRID 1105694Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1105694
Cl.Cl.C(NNCC)C.O1CC[N:12]([CH2:15][CH:16]([N+:24]([O-:26])=[O:25])[CH2:17][N:18]2CCO[CH2:20][CH2:19]2)[CH2:11][CH2:10]1>CO.C1(C)C=CC=CC=1>[N+:24]([CH:16]1[CH2:15][N:12]([CH2:11][CH3:10])[N:18]([CH2:19][CH3:20])[CH2:17]1)([O-:26])=[O:25]

Komponenten

5

Edukt 2

HCID 243721,2-Diethylhydrazine dihydrochlorideHCID 6881101,3-DIMORPHOLINO-2-NITROPROPANE

Produkt 1

HCID 10442180HCID 10442180, VerbindungAusbeute 54 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 1140TolueneLösungsmittel

Versuchsvorschrift

A stirred solution of 4.03 g (0.025 moles) of 1,2-diethylhydrazine dihydrochloride and 6.72 g. (0.026 moles) of 1,3-dimorpholino-2-nitropropane in a mixture of 28 ml of methanol and 16 ml of toluene was heated at reflux for 3 hours. The solvents were evaporated under reduced pressure and the residue was resuspended in 100 ml of toluene. The solid morpholine hydrochloride was removed by filtration, leaving a solution of 4-nitro-1,2-diethyl-pyrazolidine in solution. To the toluene solution was added 60 ml anhydrous ethanol and 2 g. of Raney Nickel which had been washed three times with anhydrous ethanol. The mixture was hydrogenated at about 30 psi. hydrogen pressure. The mixture was filtered carefully under nitrogen to prevent ignition. Evaporation of solvents and distillation at reduced pressure gave colorless liquid product weighing 1.95 g. (54% yield calculated on diethylhydrazine), b.p. 113°-115° C./40 mm.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. customThe solvents were evaporated under reduced pressure
  4. customThe solid morpholine hydrochloride was removed by filtration

Quellen und Nachweise

ORD-Eintrag
ord-5839c8a675574615ac01a9c0da5aeb9a
Quelldatensatz
uspto-grants-1982_01
Patentnummer
US04309552

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