Reaktion #318912

ord-068a47997e2c45ea9953c3a15c70f647

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturWith cooling
  2. 2
    workup.ADDITIONWhen the dropwise addition
  3. 3
    workup.STIRRINGstirring
  4. 4
    Einengenthe reaction mixture is then concentrated to dryness
  5. 5
    workup.DISTILLATIONis purified by high vacuum distillation

Vorschrift

With cooling and stirring, an ethereal diazomethane solution prepared from 3.1 g of nitrosomethylurea and aqueous sodium hydroxide solution in ether is added dropwise to a solution of 3.4 g of 2,2',4,4'-tetrachlorobenzil in 50 ml of dioxane. When the dropwise addition is complete, stirring is continued for 16 hours at room temperature, and the reaction mixture is then concentrated to dryness. The residual oil is crude 2-(2,4-dichlorobenzoyl)-2-(2,4-dichlorophenyl)oxirane which is purified by high vacuum distillation.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04849007uspto-grants-1989_07