3,6-Octanedione → HCID 23275890, Verbindung

HRID 1389998Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1389998
[NH:1]([C:3]1[N:4]=[N:5][C:6]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)=[CH:7][CH:8]=1)[NH2:2].[CH3:15][CH2:16][C:17](=O)[CH2:18][CH2:19][C:20](=O)[CH2:21][CH3:22]>C(O)(=O)C>[CH2:21]([C:20]1[N:2]([NH:1][C:3]2[N:4]=[N:5][C:6]([N:9]3[CH2:10][CH2:11][O:12][CH2:13][CH2:14]3)=[CH:7][CH:8]=2)[C:17]([CH2:16][CH3:15])=[CH:18][CH:19]=1)[CH3:22]

Komponenten

4

Edukt 2

HCID 1650543,6-OctanedioneHCID 12603548HCID 12603548, Verbindung

Produkt 1

HCID 23275890HCID 23275890, VerbindungAusbeute 85,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel2×

Reaktionsbedingungen

Temperatur
67 °C

Versuchsvorschrift

To 1.95 g (10 m moles) of 3-hydrazino-6-morpholino-pyridazine dissolved in 12 ml of acetic acid, 1.71 g (12 m moles) of 3,6-octanedione dissolved in 4 ml of acetic acid are added at room temperature. The mixture is heated at 67° C. for 2 hours and then evaporated to dryness under vacuum. The oily residue is dissolved in toluene and the solution is evaporated to dryness. The residue is slurried with ice-water and neutralized with sodium bicarbonate to yield 2.58 g of a solid product. Said material, after crystallization from isopropanol gives 1.25 g (42%) of the title product, melting at 186°-9° C. Elemental analysis, I. R., N.M.R. and mass spectra are in agreement with the assigned structure.

Aufarbeitung

  1. additionare added at room temperature
  2. customevaporated to dryness under vacuum
  3. dissolutionThe oily residue is dissolved in toluene
  4. customthe solution is evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-2577727d135a48c081c88daa4e556844
Quelldatensatz
uspto-grants-1981_01
Patentnummer
US04247551

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