反应详情

温度

75 °C

A mixture of 2,4-dihydro-4-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one (0.05 mol), ethyl 2-bromobutanoate (0.055 mol) and Na2CO3 (0.15 mol) in 1-methyl-2-pyrrolidinone (250 ml) was stirred at 75° C. overnight. Ethyl 2-bromobutanoate (0.015 mol) was added again. The mixture was stirred at 75° C. for 6 hours, at room temperature for 48 hours, poured out into H2O and stirred for 30 minutes. The precipitate was filtered off and dissolved in CH2Cl2. The solution was filtered. The filtrate was dried, filtered and the solvent was evaporated. The residue was triturated in DIPE and ethyl acetate, filtered off and dried, yielding 10 g (43%) of (±)-ethyl α-ethyl-4,5-dihydro-4-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-5-oxo-1H-1,2,4-triazol-1-acetate (interm. 9).

1. stirringThe mixture was stirred at 75° C. for 6 hours, at room temperature for 48 hours
2. stirringstirred for 30 minutes
3. filtrationThe precipitate was filtered off
4. dissolutiondissolved in CH2Cl2
5. filtrationThe solution was filtered
6. customThe filtrate was dried
7. filtrationfiltered
8. customthe solvent was evaporated
9. customThe residue was triturated in DIPE and ethyl acetate
10. filtrationfiltered off
11. customdried