Hydrochloric Acid → HCID 21186672, Verbindung

HRID 1384264Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1384264
[CH3:1][C:2]1[N:7]=[C:6]2[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:5]2=[CH:4][C:3]=1[C:13]([O:15]CC)=[O:14].Cl>[OH-].[Na+]>[CH3:1][C:2]1[N:7]=[C:6]2[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:5]2=[CH:4][C:3]=1[C:13]([OH:15])=[O:14]

Komponenten

4

Versuchsvorschrift

Ethyl 2-methyl-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carboxylate (3.05 g, 13.1 mmol) was suspended in 5% sodium hydroxide aqueous solution (20.0 ml) and heated under reflux for 1 hour. After cooling to room temperature, this was adjusted to pH 4 by adding concentrated hydrochloric acid and extracted with chloroform-methanol (4:1) mixed solvent. The thus obtained organic layer was washed with saturated brine and then dried over anhydrous sodium sulfate. By evaporating the solvent under reduced pressure, the title compound (1.95 g, 72.7%) was obtained as pale brown powder.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. extractionextracted with chloroform-methanol (4:1)
  4. additionmixed solvent
  5. washThe thus obtained organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customBy evaporating the solvent under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-76ceae29ce494296ab4dbf8d8c16e20a
Quelldatensatz
uspto-grants-2001_07
Patentnummer
US06258829B1

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