Reaktion #443414

ord-87c2af0f2e534f4e8e9b7bb2f3b95c78

Reaktionsbedingungen

Temperatur
190°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONwas fed into the twelfth step from the top of a first fifty-plate Oldershaw-type reactive distillation column
  2. 2
    Sonstigeprovided with a one liter bottom flask
  3. 3
    Sonstigewhile withdrawing a resultant vapor fraction from the top portion of the first column
  4. 4
    Sonstigeat a reflux ratio of 2 and condensing the withdrawn vapor fraction by a cooler

Vorschrift

A solution comprising 54.1% by weight of phenol, 45.3% by weight of dimethyl oxalate and 0.5% by weight of tetraphenoxytitanium was fed into the twelfth step from the top of a first fifty-plate Oldershaw-type reactive distillation column provided with a one liter bottom flask and having an inner diameter of 32 mm, at a flow rate of 600 ml/hr, and the bottom flask was heated by a mantle heater to a temperature of 190° C., while withdrawing a resultant vapor fraction from the top portion of the first column at a reflux ratio of 2 and condensing the withdrawn vapor fraction by a cooler, to transesterify dimethyl oxalate with phenol and to produce diphenyl oxalate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05834615uspto-grants-1998_11