反应详情

A mixture of 3-amino-5-mercapto-s-triazole (Compound 5) [4.64g; 40 mmoles] in 40 ml. of IN sodium hydroxide was stirred at room temperature while solution of p-chlorobenzylchloride [7.55g; 48 mmoles] in 80 ml of absolute ethanol was added. The mixture was then warmed to 70°-75° and stirred for 30 minutes. The amber colored solution was then evaporated to 40 ml at reduced pressure, diluted with 50 ml of water and chilled overnight. The crude product was separated by filtration, air dried, and recrystallized two times from chloroform to afford 4.3g (45%) of analytically pure product that had a melting point of 107°-8°.

1. additionwas added
2. temperatureThe mixture was then warmed to 70°-75°
3. customThe amber colored solution was then evaporated to 40 ml at reduced pressure
4. additiondiluted with 50 ml of water
5. temperaturechilled overnight
6. customThe crude product was separated by filtration, air
7. customdried
8. customrecrystallized two times from chloroform
9. customto afford 4.3g (45%) of analytically pure product that