反应详情

温度

90 °C

To a stirred solution of methane sulfonate (as obtained in Step (i) of Example 1) (215 mg, 0.62 mmol) in dry dimethylfuran (2 mL) was added sodium azide (180 mg, 2.77 mmol). The reaction mixture was gradually heated to 90° C. and stirred for 16 hours. Upon completion of the reaction, it was diluted with ether, washed with water, brine, dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure. The crude product was purified by silica gel flash column chromatography to obtain the title compound as gummy liquid of 164 mg. Yield: 90%.

1. customUpon completion of the reaction, it
2. washwashed with water, brine
3. dry with materialdried over anhydrous sodium sulfate
4. customthe solvent was removed under reduced pressure
5. customThe crude product was purified by silica gel flash column chromatography