Reaktion #10481

ord-1a5375979fb5402d8fe980b291f4b317

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturto reflux
  3. 3
    Temperaturat reflux until the reaction
  4. 4
    SonstigeOn completion of the reaction period
  5. 5
    Temperaturthe solution was cooled to 80–90° C.
  6. 6
    Waschenwashed with water (69 L)

Vorschrift

A mixture of purified 1-(4-methylphenyl)-1,2-cyclopropanedicarboxylic acid (58 kg), toluene (465 kg) and urea (23.8 kg) was heated to reflux and the mixture held at reflux until the reaction was complete. On completion of the reaction period, the solution was cooled to 80–90° C. and washed with water (69 L). The lower aqueous layer was discarded. In this way (±)-1-(4-methylphenyl)-3-azabicyclo[3.1.0]hexan-2,4-dione was obtained as a solution in toluene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07094799B2uspto-grants-2006_08