反应详情

To a stirred solution of isopropyl 2-[4-fluoro-3-[[2-fluoro-3-(3-fluorophenyl)-5-methyl-phenyl]methylamino]-2-methyl-phenoxy]acetate (100 mg, 0.22 mmol, 1.0 eq) in a mixture of THF (10 mL) and H2O (10 mL) was added NaOH (17 mg, 0.44 mmol, 2.0 eq). The reaction was stirred for 2 h then acidified to pH 4 by addition of 1M HCl. The aqueous layer was extracted with EtOAc and the combined organic extracts were washed with brine, dried (Na2SO4), filtered and evaporated in vacuo. The residue obtained was purified by column chromatography (CH2Cl2:MeOH, 20:1) to give a partially purified material. Further purification by preparative HPLC provided the title compound as yellow solid (9 mg, 10%).

1. extractionThe aqueous layer was extracted with EtOAc
2. washthe combined organic extracts were washed with brine
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. customevaporated in vacuo
6. customThe residue obtained
7. customwas purified by column chromatography (CH2Cl2:MeOH, 20:1)
8. customto give a partially purified material
9. customFurther purification by preparative HPLC