Water → HCID 12268076, Verbindung

HRID 585553Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 585553
[CH3:1][C:2]1([CH2:14][CH2:15][CH3:16])[CH:7](C#N)[C:6](=[O:10])N[C:4](=[O:11])[CH:3]1C#N.[OH2:17]>S(=O)(=O)(O)O>[CH3:1][C:2]1([CH2:14][CH2:15][CH3:16])[CH2:3][C:4](=[O:11])[O:17][C:6](=[O:10])[CH2:7]1

Komponenten

4

Edukt 2

HCID 962WaterHCID 9585664635-91-2

Produkt 1

HCID 12268076HCID 12268076, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

Following the procedure of Vogel, A. I.; J. Chem. Soc., 1934; 1758-1765: 4-Methyl-2,6-dioxo-4-propyl-piperidine-3,5-dicarbonitrile was dissolved in 50 mL of sulfuric acid and stirred for 16 hrs. Water (50 mL) was added and the solution was refluxed for 18 hrs. Upon cooling, the crystals were collected. The crystals were suspended in 10 mL of acetic anhydride. The suspension was heated to 130° C. and stirred for 16 hrs. The solvent was removed under reduced pressure. The residue was partitioned between saturated aqueous sodium bicarbonate and diethyl ether. The ether fraction was treated with anhydrous magnesium sulfate and concentrated under reduced pressure to give the product MS (ESI+) for C9H14O3 m/z 171.2 (M+H)+.

Aufarbeitung

  1. temperaturethe solution was refluxed for 18 hrs
  2. temperatureUpon cooling
  3. customthe crystals were collected
  4. stirringstirred for 16 hrs
  5. customThe solvent was removed under reduced pressure
  6. customThe residue was partitioned between saturated aqueous sodium bicarbonate and diethyl ether
  7. additionThe ether fraction was treated with anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customto give the product MS (ESI+) for C9H14O3 m/z 171.2 (M+H)+

Quellen und Nachweise

ORD-Eintrag
ord-4b1e42173ce342a1ad81e1f437b3a2f7
Quelldatensatz
uspto-grants-2005_08
Patentnummer
US06933304B2

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