反应详情

To a mixture of 1.47 g of N-(2,6-diisopropylphenyl)-2-(acetylthio)acetamide and 12 ml of methanol was added dropwise 1.7 ml of a 30% aqueous sodium hydroxide solution at 0° C. in an argon atmosphere. After stirring for 30 minutes, a mixture of 2.05 g of 1-bromo-12-(4-phenylpiperazinyl)dodecane synthesized in (1) above and 14 ml of methanol was added thereto, followed by stirring at 60° C. for 1 hour and then at room temperature for 16 hours. To the reaction mixture was added 100 ml of ethyl acetate, and the mixture was washed successively with water and a saturated sodium chloride aqueous solution, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to column chromatography using a 1:2 mixture of ethyl acetate and hexane as a developing solvent. The resulting crystals were recrystallized from isopropyl alcohol-water to yield 1.66 g of the title compound as white powder (m.p.=76.5° -77.5° C.).

1. stirringby stirring at 60° C. for 1 hour
2. waitat room temperature for 16 hours
3. washthe mixture was washed successively with water
4. dry with materiala saturated sodium chloride aqueous solution, and dried over magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. additiona 1:2 mixture of ethyl acetate and hexane as a developing solvent
7. customThe resulting crystals were recrystallized from isopropyl alcohol-water