Reaktion #65598

ord-354c6294b57243618b8766efc6988b2b

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas slowly added a solution
  2. 2
    Temperaturwas cooled to room temperature
  3. 3
    Sonstigeplaced in an ice bath
  4. 4
    Filtrationfiltered through a Buchner funnel
  5. 5
    SonstigeThe collected solid was dried under vacuum at a temperature of 50° C.

Vorschrift

Into a solution containing 3.0 grams (9.0 mmol) of 3-chloro-4-(4-chloro-1-naphthoxy)-2,5-dimethylaniline prepared in Part B in 25 milliliters of toluene which solution was warmed to a temperature of 50° C. and placed under a nitrogen atmosphere was slowly added a solution containing 2.5 grams (13.8 mmol) of 2-chlorobenzoyl isocyanate in 5 milliters of toluene. After stirring for 1 hour at a temperature of 50° C. the reaction mixture was cooled to room temperature, placed in an ice bath, and filtered through a Buchner funnel. The collected solid was dried under vacuum at a temperature of 50° C. to afford 3.15 grams of 1-[3-chloro-4-(4-chloro-1-naphthoxy)-2,5-dimethylpheny 1]-3-(2- chlorobenzoyl)urea as a white solid having a melting point of 187° C. Elemental analysis of the white solid indicated the following:

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05420163uspto-grants-1995_05