反应详情

To a solution of 0.1 mole N-(2-chloroethyl)-N-nitrosocarbamoylazide in 75 ml dichloromethane is added in drops at -5 degC. (°C.) under stirring within 2 hours a solution of 0.2 mole N-aminopiperidine in 20 ml of a mixture of 4 parts by volume dichloromethane and 1 part by volume n-pentane. After the addition, the stirring is continued for one hour and a whitish-yellow precipitate is obtained. Subsequently it is shaken out with the same volume of 0.1 N H2SO4. The organic phase is dried over Na2SO4 and concentrated on the rotary evaporator. From ethyl formate/n-pentane we obtain on standing in the deep freezer yellow crystals which are homogeneous in thin-layer chromatography, after recrystallization from the same solvent mixture (silicagel foils, solvent system n-pentane/diethylether/dichloromethane 5:2:2)

1. additionAfter the addition
2. customa whitish-yellow precipitate is obtained
3. dry with materialThe organic phase is dried over Na2SO4
4. concentrationconcentrated on the rotary evaporator