反应详情

温度

100 °C

N(2,2-Dimethoxyethyl)-N′-(3-iodophenyl)urea (618 mg) was dissolved in acetic acid (10 ml) and water (1 ml) and the mixture was stirred at 20° C. for 17 h and then heated to 100° C. for 0.5 h. The solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate. The solution was washed with NaHCO3 solution, dried and purified by chromatography on 10 g silica Bond Elut cartridge eluting with EtOAc-petroleum ether (1:7 to 1:1) to give the title compound (130 mg) LCMS RT=2.66 min.

1. customThe solvent was removed under reduced pressure
2. dissolutionthe residue was dissolved in ethyl acetate
3. washThe solution was washed with NaHCO3 solution
4. customdried
5. custompurified by chromatography on 10 g silica Bond Elut cartridge
6. washeluting with EtOAc-petroleum ether (1:7 to 1:1)