Reacción #343932

ord-c984bd9a0c75459e93b03c8cf25efca2

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroA flask equipped with a stirrer
  2. 2
    Temperaturathermometer, nitrogen gas tube and reflux condenser
  3. 3
    Otroto react for 6 hours at 30° C
  4. 4
    OtroAfter the reaction
  5. 5
    Otrothe organic phase was separated
  6. 6
    Secadoby drying over magnesium sulfate overnight
  7. 7
    FiltraciónAfter filtering
  8. 8
    Otrothe filtrate was evaporated in a rotary evaporator
  9. 9
    OtroThe resulting crystals were recrystallized

Procedimiento

A flask equipped with a stirrer, thermometer, nitrogen gas tube and reflux condenser was charged with 18.6 g of 4,4'-dihydroxybiphenyl and 23.0 g of trimethylamine in 50.0 g of methylene chloride. To the flask was added 26.0 g of propargyl chloroformate dropwise over one hour and the mixture was allowed to react for 6 hours at 30° C. After the reaction, the reaction mixture was treated with methylene chloride-water mixture and the organic phase was separated followed by drying over magnesium sulfate overnight. After filtering, the filtrate was evaporated in a rotary evaporator. The resulting crystals were recrystallized to give the title compound at a yield of 93.6% of theory.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05258542uspto-grants-1993_11