反应详情

Four grams of thionyl chloride is added dropwise to a solution of 10 g of 3-hydroxymethyl-4-(3-o-chlorobenzoyl-5-ethyl-2-thienyl)-5-methyl-4H-1,2,4-triazole in 50 ml of dioxane. The mixture is stirred at 70° - 80°C for 2 hours. The reaction mixture is poured into 200 ml of water and made alkaline with potassium carbonate. The oil liberated is extracted with ethyl acetate. The extract is washed with water, dried over anhydrous sodium sulfate and concentrated in vacuo. The residue is treated with ligroin containing 5% ethyl acetate to cause crystallization. The crystals are collected by suction filtration and recrystallized from ligroin containing 5% ethyl acetate to give 9.3 g of 3-chloromethyl-4-(3-o-chlorobenzoyl-5-ethyl-2-thienyl)-5-methyl-4H-1,2,4-triazole as colorless pillars melting at 109° - 110°C.

1. extractionThe oil liberated is extracted with ethyl acetate
2. washThe extract is washed with water
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated in vacuo
5. additionThe residue is treated with ligroin containing 5% ethyl acetate
6. customcrystallization
7. filtrationThe crystals are collected by suction filtration
8. customrecrystallized from ligroin containing 5% ethyl acetate