Reacción #441413

ord-5501bf9ea2dd4b519af242077d9fb38e

Disolventes

Condiciones de reacción

Temperatura
180°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaheated
  2. 2
    TemperaturaThe reaction solution was cooled
  3. 3
    OtroInsoluble matter was removed by filtration
  4. 4
    ConcentraciónThen the solvent was concentrated under reduced pressure
  5. 5
    OtroThe obtained crude product
  6. 6
    Otrowas purified on silica gel column chromatography (elution with benzene)

Procedimiento

1.07 g of 5,5-dimethoxy-1,2,3,4-tetrachlorocyclopenta-1,3-diene, 0.34 g of sodium hydrogen carbonate, 0.50g of trans-1-(3-methylisoxazol-5-yl)-1-propene and 0.05 g of hydroquinone were mixed and heated with stirring at 180° C. for 7 hours. The reaction solution was cooled and ethyl acetate was added. Insoluble matter was removed by filtration. Then the solvent was concentrated under reduced pressure. The obtained crude product was purified on silica gel column chromatography (elution with benzene) to give 0.70 g of the title compound as a mixture of isomers.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06756497B1uspto-grants-2004_06