Reacción #62744

ord-5e01e92fc0084880a6a5e07a5002bbca

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas heated
  2. 2
    Temperaturaat reflux for 4 hr
  3. 3
    Temperaturato cool
  4. 4
    OtroThe layers were separated
  5. 5
    Lavadothe ether portion was washed with water (3×250 mL and 1×100 mL)
  6. 6
    Secadodried over magnesium sulfate
  7. 7
    ConcentraciónThe ether solution was concentrated

Procedimiento

A mixture of sodium methoxide (7.02 g, 0.13 mole), 7,8-dimethoxy-5-formyl-2H-1-benzopyran (57 g, 0.26 mole) and 3-ethoxypropanenitrile (28.35 g, 0.286 mole) in methanol (150 mL) was heated at reflux for 4 hr, allowed to cool and diluted with water (150 mL) and ethylether (500 mL). The layers were separated and the ether portion was washed with water (3×250 mL and 1×100 mL) and dried over magnesium sulfate. The ether solution was concentrated to give 55 g (73%) of an amber oil which was used without further purification.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04761475uspto-grants-1988_08