Reaktion #363302

Reaktionsgleichung

KOH

2,2,6-trimethyl-6-ethyl-4-oxopiperidine

KOH

→

2,2,6-trimethyl-6-ethyl-piperidin

Ausbeute 19.3%

Lösungsmittel

water

diethylenglykol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONare added
2. 2
   workup.DISTILLATION30 ml are distilled off
3. 3
   workup.ADDITIONTo the residue two times 40 ml of water are added
4. 4
   Sonstigeremoved by distillation
5. 5
   Extraktionextracted with methyl-tert.-butylether

Vorschrift

33.8 g (0.2 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 additional amount of 30 g KOH dissolved in 30 ml water are added. 30 ml are distilled off. To the residue two times 40 ml of water are added 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-piperidin are isolated by fractionated distillation. A colorless liquid is obtained with a b. p. of 78-88° C./15 mbar.

Quelle