Reacción #477183

ord-cf875ff17b274de9991888eeaacf2388

Disolventes

Condiciones de reacción

Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.DISSOLUTIONdissolved
  2. 2
    workup.ADDITIONAfter adding
  3. 3
    OtroAfter removing ethanol
  4. 4
    workup.DISTILLATIONby distillation
  5. 5
    Filtraciónthe produced solid was filtered
  6. 6
    Otroacetic acid was completely removed
  7. 7
    Lavadoby washing with NaHCO3 twice

Procedimiento

2,3-Dioxo-1-p-tolylpiperidine-4-carbonitrile (3.56 g, 15.597 mmol) was added to anhydrous ethanol (52.0 mL) and dissolved by heating to 60° C. After adding hydrazine hydrochloride (1.06 mL, 21.836 mmol) and glacial acetic acid (1.34 mL, 23.396 mmol) room temperature, reaction was carried out for 2 days. After removing ethanol by distillation, the produced solid was filtered and then acetic acid was completely removed by washing with NaHCO3 twice or more times. A target compound (3.25 g, 13.414 mmol, 86.0%) was yielded as white solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08383631B2uspto-grants-2013_02