反应详情

A mixture of 25 parts of N,N-bis(2-chloroethyl)-4-methoxybenzenamine, 23.2 parts of 2-(4-aminophenyl)-2,4-dihydro-5-methyl-4-propyl-3H-1,2,4-triazol-3-one, 2 parts of potassium iodide and 200 parts of cyclohexanol was stirred and refluxed for 5 hours using a water-separator. The reaction mixture was cooled and neutralized with a sodium hydrogen carbonate solution. The product was filtered off and dissolved in trichloromethane. The solution was filtered over silica gel and the solvent was evaporated. The residue was crystallized from 1-butanol, yielding 18 parts (44%) of 2,4-dihydro-2-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-5-methyl-4-propyl-3H-1,2,4-triazol-3-one; mp. 202.2° C. (int. 22).

1. temperaturerefluxed for 5 hours
2. temperatureThe reaction mixture was cooled
3. filtrationThe product was filtered off
4. dissolutiondissolved in trichloromethane
5. filtrationThe solution was filtered over silica gel
6. customthe solvent was evaporated
7. customThe residue was crystallized from 1-butanol