Hydrazine hydrate (1:1) → HCID 178514446, Verbindung

HRID 1965994Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1965994
[OH:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([C:8]([O:10]CC)=O)[CH2:4][CH2:3]1.O.[NH2:14][NH2:15]>>[OH:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([C:8]([NH:14][NH2:15])=[O:10])[CH2:4][CH2:3]1

Komponenten

3

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 178472487HCID 178472487, Verbindung

Produkt 1

HCID 178514446HCID 178514446, VerbindungAusbeute 91 %

Versuchsvorschrift

A mixture of cis/trans ethyl 4-hydroxycyclohexane carboxylate (5.0 g, 29 mmol) and hydrazine hydrate (1.4 g, 29 mmol) was heated at reflux for 24 h. Residual water was removed by azeotropic distillation with toluene. The residue was triturated from tert-butyl methyl ether. The precipitate was collected by filtration and dried in vacuo to give the title compound as white solid in 91% yield.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 24 h
  3. customResidual water was removed by azeotropic distillation with toluene
  4. customThe residue was triturated from tert-butyl methyl ether
  5. filtrationThe precipitate was collected by filtration
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-4c56c742f1564801ba2776846b93bf1f
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08420633B2

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