Water → HCID 18466650, Verbindung

HRID 1601006Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1601006
[CH3:1][CH:2]([C:4](=O)[C:5](=O)[CH:6]([CH3:8])[CH3:7])[CH3:3].[CH:11]1([NH2:18])[CH2:16][CH2:15][CH2:14][CH2:13][CH:12]1[NH2:17].O>C(O)(=O)C>[CH:2]([C:4]1[C:5]([CH:6]([CH3:8])[CH3:7])=[N:18][C:11]2[CH2:16][CH2:15][CH2:14][CH2:13][C:12]=2[N:17]=1)([CH3:3])[CH3:1]

Komponenten

5

Edukt 3

HCID 962WaterHCID 46101,2-DiaminocyclohexaneHCID 1382172,5-Dimethylhexane-3,4-dione

Produkt 1

HCID 18466650HCID 18466650, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

8.7 g of 2,5-dimethyl-3,4-hexanedione and 11.2 ml of 1,2-cyclohexanediamine were dissolved in 20 ml of acetic acid. The obtained solution was heated under reflux for 30 hours, cooled by allowing to stand, and poured into water, followed by the extraction with ethyl acetate. The organic phase was washed with a saturated aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate, and concentrated in a vacuum. The obtained residue was purified by silica gel chromatography (developer: 5% ethyl acetate/hexane) to give 6.8 g of the title compound as a colorless oil.

Aufarbeitung

  1. temperatureThe obtained solution was heated
  2. temperatureunder reflux for 30 hours
  3. temperaturecooled
  4. extractionfollowed by the extraction with ethyl acetate
  5. washThe organic phase was washed with a saturated aqueous solution of sodium hydrogencarbonate
  6. dry with materiala saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate
  7. concentrationconcentrated in a vacuum
  8. customThe obtained residue was purified by silica gel chromatography (developer: 5% ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-f264a818887046ea833804579637d9d4
Quelldatensatz
uspto-grants-1999_11
Patentnummer
US05977125

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