Carbon Tetrachloride → HCID 71073515, compound

Participants

Reaction Steps

Next, 8.1 g of o-tolyl hydrazine hydrochloride and 100 mL of carbon tetrachloride were put into a 500-mL three-neck flask, 7.8 g of triethylamine (Et3N) was added dropwise to this mixture little by little, and the mixture was stirred at room temperature for 1 hour. After a predetermined time elapsed, 11 g of N-(1-ethoxybenzylidene)butyramide obtained in Step 1 was added to the mixture, and the mixture was stirred at room temperature for 24 hours. After the stirring, the mixture was dissolved in chloroform and washed with water and saturated saline. After the washing, anhydrous magnesium sulfate was added to the organic layer for drying. This mixture was gravity-filtered, and the obtained filtrate was concentrated to give an oily substance. This oily substance was purified by silica gel column chromatography. As the developing solvent, a mixed solvent of dichloromethane and ethyl acetate in a ratio of 24:1 (v/v) was used. The obtained fraction was concentrated, so that 1-(2-methylphenyl)-3-phenyl-5-propyl-1H-1,2,4-triazole (abbreviation: HPrp3tz1-mp) was obtained (a red oily substance, 45% yield). The synthesis scheme of Step 2 is shown in (A-2) below.

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