反应详情

8.7 g 1-benzyl-4-aminopiperidine, 4.6 g triethylamine and 10 g 4-nitro-2,3,5,6-tetrachloropyridine was added to 100 ml absolute dioxane and stirred for 5 hours at room temperature. After removing dioxane by distillation, the residue was taken up in methylene chloride, admixed with 2 normal hydrochloric acid and stirred vigorously for 30 min. The precipitated precipitate was separated, taken up in a small amount of water, made alkaline with 2 normal ammonia and the aqueous solution was extracted several times with dichloromethane. 13.9 g N-(1-benzylpiperidin-4-yl)-4-amino-2,3,5,6-tetrachloropyridine is obtained as an oil. TLC (mobile solvent: toluene/dioxane/water 9:4.5:0.5), Rf=0.6.

1. customAfter removing dioxane
2. distillationby distillation
3. stirringstirred vigorously for 30 min
4. customThe precipitated precipitate was separated
5. extractionthe aqueous solution was extracted several times with dichloromethane