Hydroxyamine hydrochloride → HCID 14137254, Verbindung

HRID 1075954Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1075954
[CH3:1][CH:2]1[CH2:7][CH2:6][CH:5]([CH:8]([CH3:10])[CH3:9])[C:4](=O)[CH:3]1[CH2:12][CH2:13][C:14](=O)[CH3:15].Cl.[NH2:18]O>C(O)C>[CH3:15][C:14]1[CH:13]=[CH:12][C:3]2[CH:2]([CH3:1])[CH2:7][CH2:6][CH:5]([CH:8]([CH3:10])[CH3:9])[C:4]=2[N:18]=1

Komponenten

4

Edukt 2

HCID 443297Hydroxyamine hydrochlorideHCID 141372521-Methyl-4-isopropyl-2-(3'-oxobutyl)-cyclohexan-3-one

Produkt 1

HCID 14137254HCID 14137254, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

2 g of 1-methyl-4-isopropyl-2-(3'-oxobutyl)-cyclohexan-3-one, 1.2 g of hydroxylamine hydrochloride and 100 ml of ethanol are added to a 250 ml autoclave. The autoclave is heated at 150°C for 5 hours. Thereupon, the ethanol is distilled off and the residue taken up in 40 ml of 20% potassium hydroxide solution. The mixture is extracted with diethyl ether, the extract dried over sodium sulphate and the ether subsequently distilled off. The residue is purified over a silica gel column (0.05 to 0.2 mm particles) using CHCl3 as the eluant. On distillation, there is obtained 2,5-dimethyl-8-isopropyl-5,6,7,8-tetrahydroquinoline (formula IV) with a boiling point of 70°-72°C/0.4 mm Hg.

Aufarbeitung

  1. distillationThereupon, the ethanol is distilled off
  2. extractionThe mixture is extracted with diethyl ether
  3. dry with materialthe extract dried over sodium sulphate
  4. distillationthe ether subsequently distilled off
  5. customThe residue is purified over a silica gel column (0.05 to 0.2 mm particles)
  6. distillationOn distillation

Quellen und Nachweise

ORD-Eintrag
ord-e083394cc7c44bf39deccb7efa8ca77a
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03954794

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