Reaktion #806477

Reaktionsgleichung

N-(5-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-benzamide

phosphorous oxychloride

→

title compound

5-Phenyl-3-trifluoromethyl-1H-pyrazolo[4,3-c]isoquinoline

Lösungsmittel

nitrobenzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONThe solvent was distilled off under high vacuum
2. 2
   Sonstigethe residue was partitioned between ethyl acetate and water
3. 3
   WaschenThe organic portion was washed with saturated sodium bicarbonate, water and brine
4. 4
   Trocknendried over magnesium sulphate
5. 5
   EinengenConcentration and purification by MPLC
6. 6
   Wascheneluting with 1/3 ethyl acetate/heptane

Vorschrift

A mixture of 1.02 g of N-(5-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-benzamide in 10 mL of nitrobenzene was treated with 0.41 mL of phosphorous oxychloride and stirred at 185° C. for 6 h. The solvent was distilled off under high vacuum and the residue was partitioned between ethyl acetate and water. The organic portion was washed with saturated sodium bicarbonate, water and brine and dried over magnesium sulphate. Concentration and purification by MPLC, eluting with 1/3 ethyl acetate/heptane, gave the title compound as a white solid, melting point 264–265° C.

Quelle