反应详情

To a stirred solution of [4-({[2-(benzo[1,3]dioxol-5-yloxy)-pyridine-3-carbonyl]-amino}-methyl)-3-fluoro-phenoxy]-acetic acid methyl ester (0.40 g, 0.88 mmol) in tetrahydrofuran (10 mL) and methanol (2 mL) was added aqueous lithium hydroxide (2 mL, 1 M, 2 mmol). The reaction was stirred at room temperature 1 hour. The solvents were stripped in vacuo and the residue partitioned between dilute aqueous hydrochloric acid and ethyl acetate. The aqueous was extracted with 2 aliquots ethyl acetate and the pooled organics were washed with brine, dried over sodium sulfate and concentrated in vacuo to afford a yellow solid. The crude product was recrystallized from ethyl acetate to afford 80 mg of a white crystalline solid (0.18 mmol, 21% yield). mp 180° C.

1. customthe residue partitioned between dilute aqueous hydrochloric acid and ethyl acetate
2. extractionThe aqueous was extracted with 2 aliquots ethyl acetate
3. washthe pooled organics were washed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customto afford a yellow solid
7. customThe crude product was recrystallized from ethyl acetate