반응 #1837573

반응 방정식

mixture

1-(difluoromethyl)-3-(4-fluorophenyl)-1H-pyrazole-4-carboxamide

Lawesson's reagent

→

1-(difluoromethyl)-3-(4-fluorophenyl)-1H-pyrazole-4-carbothioamide

수율 85.8%

용매

THF

반응 조건

후처리

1. 1
   온도After cooling to room temperature
2. 2
   농축the reaction mixture was concentrated under reduced pressure
3. 3
   기타The obtained residue was purified by silica gel column chromatography (solvent; 7% ethyl acetate/hexane)

실험 절차

To a solution of the mixture (1.15 g, 4.51 mmol) obtained in step 3 in THF (18.8 mL) was added Lawesson's reagent (1.46 g, 3.61 mmol) at room temperature, and the mixture was stirred at 60° C. for 3 hr. After cooling to room temperature, and the reaction mixture was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (solvent; 7% ethyl acetate/hexane) to give a mixture (0.840 g, 68%, 1:1.92 mol/mol) of 1-(difluoromethyl)-3-(4-fluorophenyl)-1H-pyrazole-4-carbothioamide and 1-(difluoromethyl)-5-(4-fluorophenyl)-1H-pyrazole-4-carbothioamide as a pale-green powder.

출처