Triethylamine → HCID 74043786, Verbindung

HRID 233664Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 233664
[CH2:1]([O:3][C:4]([N:6]1[CH2:17][CH2:16][C:9]2([O:13][CH:12]([CH3:14])[C:11](=O)[CH2:10]2)[CH2:8][CH2:7]1)=[O:5])[CH3:2].C(N(CC)CC)C.Cl.[NH2:26][OH:27]>C(O)C>[CH2:1]([O:3][C:4]([N:6]1[CH2:17][CH2:16][C:9]2([O:13][CH:12]([CH3:14])[C:11](=[N:26][OH:27])[CH2:10]2)[CH2:8][CH2:7]1)=[O:5])[CH3:2]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 4588469ethyl 2-methyl-3-oxo-1-oxa-8-azaspiro[4.5]decane-8-carboxylate

Produkt 1

HCID 74043786HCID 74043786, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

8-Ethoxycarbonyl-2-methyl-1-oxa-8-azaspiro [4.5 ]decan-3-one (20 g, 0.083 mol) was dissolved in absolute ethanol (1 L) and combined with triethylamine (11.5 ml) and hydroxylamine hydrochloride (5.7 g). The mixture was stirred at room temperature overnight. The ethanol was evaporated in vacuo and the residue was stirred with ether. The insoluble solids were filtered and the ether filtrate was evaporated. The residual oxime was purified by chomatography on silica gel and elution with ammoniated 2-10% MeOH/CHCl3. Evaporation of the solvents afforded the oxime, 11.5 g.

Aufarbeitung

  1. customThe ethanol was evaporated in vacuo
  2. stirringthe residue was stirred with ether
  3. filtrationThe insoluble solids were filtered
  4. customthe ether filtrate was evaporated
  5. customThe residual oxime was purified by chomatography on silica gel and elution with ammoniated 2-10% MeOH/CHCl3
  6. customEvaporation of the solvents

Quellen und Nachweise

ORD-Eintrag
ord-1398110263c94ba1b859a00c3558815e
Quelldatensatz
uspto-grants-1997_01
Patentnummer
US05594000

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