反应详情

温度

40 °C

In a mixture of DME (120 ml) and ethanol (12 ml) was dissolved 7-[4-(4-chlorobenzoyl)benzyl]-3,5-dimethyl-2-methylthio-7H-pyrrolo[2,3-d]pyrimidin-4(3H)-one (800 mg) followed by addition of acetic acid (672 mg), and the mixture was warmed to 40° C. Then, Raney nickel was added until disappearance of the starting compound had been verified by TLC. The catalyst was then filtered off and the solvent was distilled off under reduced pressure. The residue was dissolved in ethyl acetate, washed with saturated aqueous NaHCO3 solution and saturated aqueous NaCl solution in that order, and dried over anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure and the residue was allowed to stand, whereupon crystals separated out. This crystal crop was harvested by filtration, rinsed with ethanol and hexane, and dried to provide the title compound (608 mg).

1. filtrationThe catalyst was then filtered off
2. distillationthe solvent was distilled off under reduced pressure
3. dissolutionThe residue was dissolved in ethyl acetate
4. washwashed with saturated aqueous NaHCO3 solution and saturated aqueous NaCl solution in that order
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationThe solvent was then distilled off under reduced pressure
7. customseparated out
8. filtrationThis crystal crop was harvested by filtration
9. washrinsed with ethanol and hexane
10. customdried