反应详情

温度

30 °C

1-bromoethyl acetate (700 mg, 1.7 mmol, 1.0 eq) was dissolved in DMA (10 mL) at room temperature. K2CO3 (120 mg, 0.9 mmol, 0.5 mmol) was added and the mixture stirred for 90 min at 30° C. under a nitrogen atmosphere. The reaction was cooled to −5° C. and 2-[2,4-difluoro-3-[[2-fluoro-5-(3-fluorophenyl)phenyl]methylamino]phenoxy]acetic acid (I(b)) (350 mg, 2.1 mmol, 1.2 eq) was added. The reaction was warmed to 30° C. over 30 min and stirred for a further 30 min. The reaction was quenched by addition of water and extracted with ethyl acetate. The organic extract was dried (Na2SO4), filtered and evaporated in vacuo and the residue obtained purified by column chromatography (petroleum ether: EtOAc, 10:1) to give the title compound as a colourless oil (200 mg, 23%).

1. temperatureThe reaction was cooled to −5° C.
2. temperatureThe reaction was warmed to 30° C. over 30 min
3. stirringstirred for a further 30 min
4. customThe reaction was quenched by addition of water
5. extractionextracted with ethyl acetate
6. extractionThe organic extract
7. dry with materialwas dried (Na2SO4)
8. filtrationfiltered
9. customevaporated in vacuo
10. customthe residue obtained
11. custompurified by column chromatography (petroleum ether: EtOAc, 10:1)