Methanol → Sodium 6-(4-ethylpiperazinyl)pyridine-3-carboxylate

HRID 1003316Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1003316
[OH-].[Na+:2].CO.[CH2:5]([N:7]1[CH2:12][CH2:11][N:10]([C:13]2[N:18]=[CH:17][C:16]([C:19]([O:21]C)=[O:20])=[CH:15][CH:14]=2)[CH2:9][CH2:8]1)[CH3:6]>O>[CH2:5]([N:7]1[CH2:8][CH2:9][N:10]([C:13]2[N:18]=[CH:17][C:16]([C:19]([O-:21])=[O:20])=[CH:15][CH:14]=2)[CH2:11][CH2:12]1)[CH3:6].[Na+:2]

Komponenten

5

Edukt 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 14987929Methyl 6-(4-ethylpiperazin-1-yl)nicotinate

Produkt 1

HCID 23663821Sodium 6-(4-ethylpiperazinyl)pyridine-3-carboxylateAusbeute 111,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 3.1 g of sodium hydroxide in 15 ml of water was added to 75 ml of methanol. 15 g of methyl 6-(4-ethyl-1-piperazinyl)pyridine-3-carboxylate was added and the mixture was heated under reflux for 1.5 hours. The solvent was distilled off under reduced pressure, to the resulting residue was added hot acetone and the crystal thus precipitated out was recovered by filtration. It was again washed with hot acetone to afford 17.2 g of the title compound as a crystal.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. distillationThe solvent was distilled off under reduced pressure, to the resulting residue
  4. additionwas added hot acetone
  5. customthe crystal thus precipitated out
  6. filtrationwas recovered by filtration
  7. washIt was again washed with hot acetone

Quellen und Nachweise

ORD-Eintrag
ord-9f1225e7359d460ea87081127b400aa0
Quelldatensatz
uspto-grants-2000_04
Patentnummer
US06046201

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