反应详情

温度

70 °C

A mixture of 5 parts of 1,3-dihydro-1-(3-iodopropyl)-3-methyl-2H-benzimidazol-2-one, 3,4 parts of 1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one, 2.65 parts of sodium carbonate and 22.5 parts of N,N-dimethylformamide is stirred and heated for 2 hours at 70° C. The reaction mixture is cooled and poured onto water, whereupon an oily precipitate is formed. The supernatant aqueous phase is decanted and the residual oil is dissolved in trichloromethane. The solution is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 5% of methanol as eluent. The pure fractions are collected and the eluent is evaporated, yielding 1 part of 8-[3-(1,3-dihydro-3-methyl-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one; mp. 164.4° C.

1. temperatureThe reaction mixture is cooled
2. additionpoured onto water, whereupon an oily precipitate
3. customis formed
4. customThe supernatant aqueous phase is decanted
5. dissolutionthe residual oil is dissolved in trichloromethane
6. customThe solution is dried
7. filtrationfiltered
8. customevaporated
9. customThe residue is purified by column-chromatography over silica gel using
10. additiona mixture of trichloromethane and 5% of methanol as eluent
11. customThe pure fractions are collected
12. customthe eluent is evaporated