Reacción #63155

ord-cad2be3f15de4c6eaa93a331efc5ead5

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwas added portionwise at a rate
  2. 2
    Temperaturato maintain a reflux temperature of about 130°-135° C
  3. 3
    TemperaturaThe mixture was refluxed an additional two hours
  4. 4
    Filtraciónfiltered
  5. 5
    Concentraciónthe filtrate was concentrated in vacuo

Procedimiento

A suspension of 8 g of the product of Example 7 and 0.4 g of DABCO in 90 ml of xylenes was heated under N2 at 130°-135° C. while 1.8 ml of phosgene was added portionwise at a rate to maintain a reflux temperature of about 130°-135° C. The mixture was refluxed an additional two hours, cooled under N2 to room temperature, filtered, and the filtrate was concentrated in vacuo to yield 6.9 g of the subject compound as a crude oil.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04764205uspto-grants-1988_08