反应详情

A mixture of 15 parts of 1-(4-fluoro-2-nitrobenzoyl)-aziridine, 12 parts of 1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one, 8.8 parts of methanol and 56 parts of benzene is stirred first for 1.50 hours at reflux and further overnight at room temperature. The reaction mixture is evaporated. The residue is dissolved in trichloromethane and the solution is washed with water. Then there are added 8 parts of methanol and silica gel and the whole is stirred for 10 minutes. The silica gel is filtered off and the filtrate is evaporated. The residue is stirred in 2,2'-oxybispropane. The product is filtered off and crystallized from 4-methyl-2-pentanone. It is filtered off and dried, yielding 13 parts of 4-fluoro-2-nitro-N-[2-(4-oxo-1-phenyl-1,3,8-triazaspiro-[4,5]dec-8-yl)ethyl]benzamide; mp. 160° C.

1. customThe reaction mixture is evaporated
2. dissolutionThe residue is dissolved in trichloromethane
3. washthe solution is washed with water
4. additionThen there are added 8 parts of methanol and silica gel
5. stirringthe whole is stirred for 10 minutes
6. filtrationThe silica gel is filtered off
7. customthe filtrate is evaporated
8. stirringThe residue is stirred in 2,2'-oxybispropane
9. filtrationThe product is filtered off
10. customcrystallized from 4-methyl-2-pentanone
11. filtrationIt is filtered off
12. customdried