反应详情

To a solution of 2,4-difluoro-3-[[3-(3-fluorophenyl)-5-methoxy-phenyl]methylamino]phenol (see example 16) (1.0 g, 2.78 mmol, 1.0 eq) in DMF (10 mL) was added Cs2CO3 (1.36 g, 3.34 mmol, 1.5 eq) at room temperature. The reaction mixture was stirred for 1 h, then isopropyl 2-bromoacetate (624 mg, 3.34 mmol, 1.2 eq) was added and the reaction mixture was stirred for h. The resulting mixture was poured into water and extracted with EtOAc. The organic extract was washed with water and brine, dried (Na2SO4) and evaporated in vacuo. The residue obtained was purified by column chromatography, (EtOAc:petroleum ether 0:1 to 1:20) to give the title compound as a colourless oil (0.8 g, 62%).

1. stirringthe reaction mixture was stirred for h
2. extractionextracted with EtOAc
3. extractionThe organic extract
4. washwas washed with water and brine
5. dry with materialdried (Na2SO4)
6. customevaporated in vacuo
7. customThe residue obtained
8. customwas purified by column chromatography, (EtOAc:petroleum ether 0:1 to 1:20)