Reaktion #836501

ord-18b99433c5754879a6932717b073ad81

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATION30 ml are distilled off
  2. 2
    Sonstigeremoved by distillation
  3. 3
    Extraktionextracted with methyl-tert.-butylether

Vorschrift

33.8 g (02 mol) 2,2,6-trimethyl-6-ethyl-4-oxopiperidine, 14 g (0.28 mol) hydrazinhydrate and 13 g KOH in 80 ml diethylenglykol are stirred for 4 h at 160° C. Subsequently an aciditional amount of 30 g KOH dissolved In 30 ml water are acided. 30 ml are distilled off. To the residue two times 40 ml of water are acided and removed by distillation. The combined distillates are saturated with solid K2CO3 and extracted with methyl-tert.-butylether. From the extracts 6 g ( 19%) 2,2,6-trimethyl-6-ethyl-piperidine are isolated by fractionated distillation. A colorless liquid is obtained with a b. p. of 78-88° C./15 mbar.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07402639B2uspto-grants-2008_07