Potassium Hydroxide → HCID 22341853, compound

HRID 749319Notes

Reaction equation

HRID 749319 reaction equation
[CH3:1][C:2]1([CH3:12])[CH2:7][C:6](=O)[CH2:5][C:4]([CH3:11])([CH2:9][CH3:10])[NH:3]1.[OH-].[K+]>C(O)COCCO.O>[CH3:1][C:2]1([CH3:12])[CH2:7][CH2:6][CH2:5][C:4]([CH3:11])([CH2:9][CH3:10])[NH:3]1

Participants

5

Reactant 2

HCID 14797Potassium Hydroxide2×HCID 14961659HCID 14961659, compound

Product 1

HCID 22341853HCID 22341853, compoundYield 19.4%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8117Diethylene GlycolSolvent

Procedure

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.

Workup

  1. distillation30 ml are distilled off
  2. customremoved by distillation
  3. extractionextracted with methyl-tert.-butylether

Sources & evidence

ORD record
ord-18b99433c5754879a6932717b073ad81
Source dataset
uspto-grants-2008_07
Patent number
US07402639B2

Reaction notes

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