反应详情

To a solution of methyl N-[3-(4-phenyl-1-piperazinyl)propyl]dithiocarbamate (12.9 g) in a mixture of water (20 m) and ethanol (30 m) was added sodium azide (3.6 g). The resulting mixture was refluxed with stirring for 4.5 hours. The reaction mixture was concentrated under reduced pressure. After the addition of water to the residue, the mixture was washed successively with ethyl acetate and diethyl ether and then evaporated. To the residue was added ethanol (100 m) and the mixture was filtered. The filtrate was evaporated under reduced pressure. The residue was recrystallized from isopropyl alcohol twice to give 1-[3-(4-phenyl-1-piperazinyl)propyl]-4,5-dihydro-1H-tetrazole-5-thione (3.2 g), mp. 200° to 205° C.

1. temperatureThe resulting mixture was refluxed
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additionAfter the addition of water to the residue
4. washthe mixture was washed successively with ethyl acetate and diethyl ether
5. customevaporated
6. additionTo the residue was added ethanol (100 m)
7. filtrationthe mixture was filtered
8. customThe filtrate was evaporated under reduced pressure
9. customThe residue was recrystallized from isopropyl alcohol twice