Reacción #2254218

ord-b14ece93e0a243089b140a347f7152d3

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe solution was refluxed for 3 h
  2. 2
    OtroThe solvent removed
  3. 3
    Otrothe residue was purified on 25 g Biotage snap column
  4. 4
    Lavadoeluted with 0-18% EtOAc in Hex (12CV)

Procedimiento

A solution of [9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]hydrazine (250 mg, 1.0 mmol) in 4 mL of i-PrOH were added Et3N and 3-dimethylaminoacrolein. The solution was refluxed for 3 h and then at 50° C. for 2 d. The solvent removed and the residue was purified on 25 g Biotage snap column, eluted with 0-18% EtOAc in Hex (12CV) to give 1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole (80 mg, 31% yield).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09044469B2uspto-grants-2015_06