反应详情

温度

55 °C

A mixture of acetic anhydride (0.30 ml) and formic acid (0.13 ml) was stirred at 50-60° C. for 1 hr. To the obtained acetic formic anhydride was added a solution of 2-(4-(4-(aminomethyl)phenylmethyl)piperazin-1-yl)pyrimidin (0.42 g) in methylene chloride (10 ml) under ice-cooling and the mixture was stirred at 5-10° C. for 2 hr. The reaction mixture was concentrated under reduced pressure and the obtained residue was purified by silica gel column chromatography (developing solvent; chloroform:methanol=9:1) to give a yellow oil. (0.46 g). The obtained yellow oil was crystallized from ethyl acetate/diisopropyl ether to give the title compound (0.45 g) as pale-yellow crystals, m.p.=97-98° C.

1. temperaturecooling
2. stirringthe mixture was stirred at 5-10° C. for 2 hr
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. customthe obtained residue was purified by silica gel column chromatography (developing solvent; chloroform:methanol=9:1)
5. customto give a yellow oil
6. customThe obtained yellow oil was crystallized from ethyl acetate/diisopropyl ether