Reaktion #569809

ord-25d1f06862ae4ebdb00001cad256d452

Lösungsmittel

Reaktionsbedingungen

Temperatur
-20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenthe mixture was concentrated in vacuo
  2. 2
    workup.DISSOLUTIONdissolved in 200 ml of 50/50 diethyl ether/hexanes

Vorschrift

To an ether solution of 3-(4-propoxyphenyl)-4-(N-propyl-N-(2,2,2-trichloroethoxycarbonyl)amino)-4,5-dihydro-1H-pyrazole (Example 585e) (≤85 mmole) was added 12.7 g (68 mmole) of 4-trifluoromethylphenyl isocyanate. After stirring for 30 minutes, the mixture was concentrated in vacuo and dissolved in 200 ml of 50/50 diethyl ether/hexanes and cooled to -20° C. Crystals of the desired compound formed and were filtered yielding 23 g of the desired compound, mp 162°-163° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05798311uspto-grants-1998_08