反应详情

温度

130 °C

A mixture of 53 parts of N-{4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl}hydrazinecarboxamide, 53 parts of ethanimidamide hydrochloride and 135 parts of N,N-dimethylformamide is stirred and heated for 3 hours at 130° C. The reaction mixture is cooled and poured onto water. The precipitated product is filtered off, washed with water and with methanol, and crystallized from N,N-dimethylformamide. The product is filtered off and recrystallized from 1,4-dioxane, yielding 19.5 parts of 2,4-dihydro-4-{4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl}-5-methyl-3H-1,2,4-triazol-3-one; 298.4° C.

1. temperatureThe reaction mixture is cooled
2. additionpoured onto water
3. filtrationThe precipitated product is filtered off
4. washwashed with water and with methanol
5. customcrystallized from N,N-dimethylformamide
6. filtrationThe product is filtered off
7. customrecrystallized from 1,4-dioxane