Reaktion #657257

ord-852f47be86574ff68e08c58c5bd293f0

Reaktionsgleichung

CCOCc1cnn(C(c2ccccc2)(c2ccccc2)c2ccccc2)c1
1-trityl-4-ethoxymethylpyrazole
CCOCc1cn[nH]c1
4-ethoxymethylpyrazole
Ausbeute 44.0%

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added to the resulting solution
  2. 2
    TemperaturAfter cooling to room temperature
  3. 3
    Filtrationthe reaction mixture was filtered
  4. 4
    Waschenwashed with dichloromethane
  5. 5
    Extraktionextracted with dichloromethane
  6. 6
    Trocknendried over MgSO4
  7. 7
    Sonstigethe solvent was evaporated under vacuum

Vorschrift

1-trityl-4-ethoxymethylpyrazole (1.800 g, 4.88 mmol) was dissolved in a mixture of ethanol/acetone (15 ml/5 ml) and 30 mL of 2N HCl was added to the resulting solution. The mixture was heated at 80° C. for 2 h. After cooling to room temperature, the reaction mixture was filtered and washed with dichloromethane. The aqueous layer was basified with 2N NaOH and extracted with dichloromethane. The organic layers were combined, dried over MgSO4 and the solvent was evaporated under vacuum yielding compound 4-ethoxymethylpyrazole as a white oil. Yield: 44% (270 mg, 2.14 mmol).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09023315B2uspto-grants-2015_05