HRID1732147
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
3-Chloromethyl-1,2,4-triazole hydrochloride (0.5 g.) was added to piperidine (10 ml.) and the mixture was heated at 100° for 16 hours, then evaporated to dryness. The residue was dissolved in water (10 ml.) and basified with sodium bicarbonate. The resulting solution was evaporated to dryness and the residue was extracted twice with ethanol (50 ml.). The combined extracts were evaporated to dryness and the residual gum was subjected to MPLC on K60 silica gel using methanol/chloroform, 3/97 v/v, as solvent to give 3-(piperidinomethyl)-1,2,4-triazole with NMR data as follows: solvent--CDCl3 : 8.05 ppm (singlet, 1H), 3.75 ppm (singlet, 2H), 2.5 ppm (multiplet, 4H) and 1.6 ppm (multiplet, 6H).
WORKUP
后处理
- temperaturethe mixture was heated at 100° for 16 hours
- customevaporated to dryness
- dissolutionThe residue was dissolved in water (10 ml.)
- customThe resulting solution was evaporated to dryness
- extractionthe residue was extracted twice with ethanol (50 ml.)
- customThe combined extracts were evaporated to dryness