反应详情

温度

55 °C

A mixture of acetic anhydride (0.36 ml) and formic acid (0.15 ml) was stirred at 50-60° C. for 2 hr, and to the obtained acetic acid and formic acid anhydride was added a solution of 4-((4-(aminomethyl)phenyl)methyl)-1-phenylpiperazine (0.5 g) in methylene chloride (10 ml) under ice-cooling. This reaction mixture was stirred at 5-10° C. for 2.5 hr and left standing at room temperature for 14 hr. To this reaction mixture were added ethanol (20 ml) and ethyl acetate (150 ml) and the mixture was washed with saturated sodium hydrogencarbonate solution and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated to give a brown solid (0.56 g). The obtained solid was purified by silica gel column chromatography (developing solvent; chloroform:methanol=9:1) to give a pale-brown solid (0.55 g). The obtained solid was crystallized from ethyl acetate-hexane (2:1) to give the title compound (0.41 g) as pale-yellow white crystals, m.p.=108-109° C.

1. temperaturecooling
2. stirringThis reaction mixture was stirred at 5-10° C. for 2.5 hr
3. waitleft
4. waitstanding at room temperature for 14 hr
5. washthe mixture was washed with saturated sodium hydrogencarbonate solution and saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was evaporated