Potassium Hydroxide → HCID 22341853, compound

HRID 276120Notes

Reaction equation

HRID 276120 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 19.3%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8117Diethylene GlycolSolvent

Procedure

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.

Workup

  1. additionare added
  2. distillation30 ml are distilled off
  3. additionTo the residue two times 40 ml of water are added
  4. customremoved by distillation
  5. extractionextracted with methyl-tert.-butylether

Sources & evidence

ORD record
ord-c0d896bc92ac4d4a9c4c1201d67bd688
Source dataset
uspto-grants-2002_03
Patent number
US06353107B1

Reaction notes

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