反应详情

To a solution of (5-phenoxymethyl-pyridin-2-yl)-methanol described in Preparation Example 187 (167 mg, 0.776 mmol) in tetrahydrofuran (4 mL) were added phthalimide (126 mg, 0.856 mmol), triphenylphosphine (244 mg, 0.930 mmol) and diethyl azodicarboxylate (424 μL, 0.931 mmol, 40% toluene solution) at 0° C., and the solution was stirred at room temperature for 30 minutes. The reaction solution was partitioned with water and ethyl acetate. The organic layer was separated, washed with brine, and then, dried over anhydrous magnesium sulfate. The organic layer was filtered, then, the solvent was evaporated in vacuo, the residue was purified by silica gel column chromatography (heptane/ethyl acetate=1/1), and the title compound (383 mg, quantitatively) was obtained as a white solid.

1. customThe reaction solution was partitioned with water and ethyl acetate
2. customThe organic layer was separated
3. washwashed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationThe organic layer was filtered
6. customthe solvent was evaporated in vacuo
7. customthe residue was purified by silica gel column chromatography (heptane/ethyl acetate=1/1)