反应详情

温度

50 °C

Reaction under N2 atmosphere. NaH 60% (0.12 mol) was added to 2,4-dihydro-4-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one (0.1 mol) in DMF, and stirred for 30 minutes at 50° C. A solution of 1-chloro-2-propanone (0.1 mol) in DMF was added dropwise and the resulting reaction mixture was stirred overnight at 50° C. The reaction mixture was cooled, poured out into ice-water and the resulting precipitate was filtered off, washed with water, and dried. This fraction was recrystallized from CH2Cl2/CH3OH. The precipitate was filtered off and the filtrate was evaporated. The residue was crystallized from methanol, filtered off and dried. The residue was combined with the crystallized compound, recrystallized from CH2Cl2/CH3OH, filtered off and dried, yielding 0.65 g of 2,4dihydro-4-[4-[4-(4-methoxy-phenyl)-1-piperazinyl]phenyl]-2-(2-oxopropyl)-3H-1,2,4-triazol-3-one (interm. 20).

1. customReaction under N2 atmosphere
2. customthe resulting reaction mixture
3. stirringwas stirred overnight at 50° C
4. temperatureThe reaction mixture was cooled
5. filtrationthe resulting precipitate was filtered off
6. washwashed with water
7. customdried
8. customThis fraction was recrystallized from CH2Cl2/CH3OH
9. filtrationThe precipitate was filtered off
10. customthe filtrate was evaporated
11. customThe residue was crystallized from methanol
12. filtrationfiltered off
13. customdried
14. customrecrystallized from CH2Cl2/CH3OH
15. filtrationfiltered off
16. customdried