反应详情

After heating and dissolving the free base (2.00 kg, 3.98 mol) of 2-[4-[2-(benzimidazol-2-ylthio)ethyl]piperazin-1-yl]-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]acetamide and pyridine hydrochloride (0.92 kg, 7.96 mol) in ethanol (12 L) at reflux temperature, water (20 L) was added dropwise to the reaction mixture at 75 to 87° C. The reaction mixture was allowed to cool down to room temperature, and was stirred for 1 hour. Precipitated crystals were collected by filtration. The crystals were washed with water and dried at 80° C. under reduced pressure to obtain 2-[4-[2-(benzimidazol-2-ylthio)ethyl]piperazin-1-yl]-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]acetamide monohydrochloride water adduct (1.96 kg, 89.0%; found to contain 2% of ethanol from 1H-NMR) as colorless needles.

1. temperatureAfter heating
2. additionwas added dropwise to the reaction mixture at 75 to 87° C
3. customPrecipitated crystals
4. filtrationwere collected by filtration
5. washThe crystals were washed with water
6. customdried at 80° C. under reduced pressure