反应详情

温度

50 °C

10 Parts of 2,4-dihydro-4-{4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl}-3H-1,2,4-triazol-3-one are dissolved in 300 parts of dimethyl sulfoxide at 100° C. Then there are added 1.6 parts of sodium hydride dispersion 50% and stirring is continued while the mixture is allowed to cool to about 50° C. 3.9 Parts of 1-bromopropane are added and the whole is stirred overnight at room temperature. The reaction mixture is poured onto water and the product is extracted with trichloromethane. The extract is washed with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is triturated in 2-propanol. The product is filtered off and dried; yielding 7.5 parts (65%) of 2,4-dihydro-4-{4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl}-2-propyl-3H-1,2,4 -triazol-3-one.

1. stirringthe whole is stirred overnight at room temperature
2. additionThe reaction mixture is poured onto water
3. extractionthe product is extracted with trichloromethane
4. washThe extract is washed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe residue is purified by column-chromatography over silica gel using
9. additiona mixture of trichloromethane and methanol (98:2 by volume) as eluent
10. customThe pure fractions are collected
11. customthe eluent is evaporated
12. customThe residue is triturated in 2-propanol
13. filtrationThe product is filtered off
14. customdried