反应详情

A solution of the compound (4.00 g, 15.31 mmol) obtained in step 3 and Lawesson's reagent (6.19 g, 15.31 mmol) in THF (50 mL) was stirred at 50° C. for 1.5 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by NH-silica gel column chromatography (solvent gradient; 2→65% ethyl acetate/hexane) to give 1-tert-butyl-5-(4-fluorophenyl)-1H-pyrazole-4-carbothioamide (2.75 g, 9.91 mmol, 65%) as a pale-yellow powder.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customthe residue was purified by NH-silica gel column chromatography (solvent gradient; 2→65% ethyl acetate/hexane)