反应详情

A mixture of 3.75 parts of N-(2-chloroethyl)-1-methyl-1H-pyrrole-2-carboxamide, 5 parts of 1-(4-fluorophenyl)-1,3,8-triazaspiro[4,5]decan-4-one, 1.7 parts of sodium hydrogen carbonate, 0.1 parts of potassium iodide and 160 parts of 4-methyl-2-pentanone is stirred and refluxed for 48 hours. The reaction mixture is cooled and the solvent is evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is converted into the hydrochloride salt in 2-propanol and 2,2'-oxybispropane. The salt is filtered off and crystallized from methanol, yielding 0.8 parts of N-{2-[1-(4-fluorophenyl)-4-oxo-1,3,8-triazaspiro[4,5]dec-8-yl] ethyl} -1-methyl-1H-pyrrole-2-carboxamide hydrochloride; mp. 273.4° C.

1. temperaturerefluxed for 48 hours
2. temperatureThe reaction mixture is cooled
3. customthe solvent is evaporated
4. customThe residue is purified by column-chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
6. customThe pure fractions are collected
7. customthe eluent is evaporated
8. filtrationThe salt is filtered off
9. customcrystallized from methanol