反应详情

温度

22 °C

To a stirred solution of Intermediate 9 (0.05 g) was added a solution of 3,4-dichlorobenzoyl chloride (42.7 mg) in N,N-dimethylformamide (7 ml). The mixture was stirred at 22° C. for 15 h before the solvent was evaporated in vacuo. The residue was purified by eluting through a 1 g silica solid phase extraction cartridge (Varian Bondelut), eluting sequentially with dichloromethane, ether, ethyl acetate, acetone, acetonitrile and methanol, to give the title compound as a white solid (0.080 g). LC/MS (System A) Rt 3.10 min, Mass Spectrum m/z 442 [MH+].

1. customwas evaporated in vacuo
2. customThe residue was purified
3. washby eluting through a 1 g silica solid phase extraction cartridge (Varian Bondelut)
4. washeluting sequentially with dichloromethane, ether, ethyl acetate, acetone, acetonitrile and methanol