反应详情

To a stirred solution of ethyl 2-[3-[[2-fluoro-5-(3-fluorophenyl)phenyl]methylamino]phenoxy]acetate (317.0 mg, 0.83 mmol, 1.0 eq) in a mixture of THF (6 mL) and H2O (6 mL) was added LiOH.H2O (134 mg, 3.19 mmol, 4.0 eq). The reaction was stirred at room temperature for 1 h, then diluted with water (30 mL) and the solution neutralized by addition of 1M HCl. The mixture was extracted with EtOAc, the combined organic extracts were washed with brine, dried (Na2CO3), filtered and evaporated in vacuo. The residue obtained was triturated with petroleum ether and EtOAc (2:1) and the solid that formed collected by filtration, washed with petroleum ether:EtOAc (2:1) and dried to give the title compound I(a) as an off-white solid (200 mg, 68%).

1. extractionThe mixture was extracted with EtOAc
2. washthe combined organic extracts were washed with brine
3. dry with materialdried (Na2CO3)
4. filtrationfiltered
5. customevaporated in vacuo
6. customThe residue obtained
7. customwas triturated with petroleum ether and EtOAc (2:1)
8. customthe solid that formed
9. filtrationcollected by filtration
10. washwashed with petroleum ether:EtOAc (2:1)
11. customdried