Benzoylhydrazine → HCID 68380230, compound

Participants

Reaction Conditions

Reaction Steps

In a 200 mL three-neck flask were put 13 g (50 mmol) of N-(9H-fluoren-2-yl)isobutyrthioamide, 8.2 g (60 mmol) of benzoylhydrazine, and 70 mL of 1-butanol, and the mixture was heated and refluxed at 130° C. for 10 hours. After that, the solid in the reaction mixture was removed by suction filtration. The resulting filtrate was concentrated to precipitate a solid. After that, 1-buthanol was distilled off to precipitate a solid. The precipitated solid was removed by suction filtration, and the filtrate was purified by silica gel column chromatography. A mixed solvent of ethyl acetate and toluene (ethyl acetate: toluene=1:1) was used as a developing solvent. The resulting fraction was concentrated to give a solid. The obtained solid was recrystallized from ethyl acetate to give 1.3 g of a white solid of 4-(9H-fluoren-2-yl)-5-isopropyl-3-phenyl-4H-1,2,4-triazole in a yield of 7%. The synthesis scheme of Step 3 is shown in (c-3) below.

Provenance & Evidence