反应详情

Sodium azide (65 g; 1.0 mol), 4-phenyl-1-(2-cyanoethyl)-piperazine (215 g; 1.0 mol), and morpholine hydrochloride (124 g; 1.0 mol) were dissolved in 1 liter of morpholine, and heated at 120°-125° C with stirring for 4 hours. After the reaction mixture was allowed to cool to room temperature, it was filtered, and the solvent was removed in vacuo. The residue was mixed in water, and the pH of the resulting solution was adjusted to 5. Crude 5-[(4-phenyl-1-piperazyl)ethyl]tetrazole was collected by filtration and was dried; yield -- 170 g. The crude product was recrystallized from water and dried; yield -- 155 g (60% yield; m.p. 190°-194° C).

1. temperatureheated at 120°-125° C
2. filtrationit was filtered
3. customthe solvent was removed in vacuo
4. additionThe residue was mixed in water
5. filtrationCrude 5-[(4-phenyl-1-piperazyl)ethyl]tetrazole was collected by filtration
6. customwas dried
7. customThe crude product was recrystallized from water
8. customdried