Reaktion #569811

ord-298edea4f19645388b55eff9618c32a9

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenthe reaction mixture was washed with water and brine
  2. 2
    Einengenconcentrated in vacuo
  3. 3
    Sonstigechromatographed over silica gel

Vorschrift

To 3.0 g (6.7 mmole) of N-(4-trifluoromethylphenyl)-3-(4-propoxyphenyl)-4-(N-propylamino)-4,5,-dihydro-1H-pyrazole-1-carboxamide (Example 586) dissolved in 25 ml of ethyl acetate and cooled to 0° C., was added 2.4 g (30 mmole) of pyridine and 4.0 g (28 mmole) of formic acetic anhydride mixture (Example 621a). After 30 minutes, the reaction mixture was washed with water and brine, concentrated in vacuo, and chromatographed over silica gel using hexanes and ethyl acetate to yield 2.5 g of the desired compound, mp 161°-163° C.

Quelle

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