反应详情

To a 100 mL flask was added tetra-n-butyl ammonium phosphoric acid di-tert-butyl ester salt (3.08 g, 6.8 mmol), ethylene glycol dimethyl ether (10 mL), and 3-bromo-1-propanol (freshly distilled from potassium carbonate). The reaction mixture was heated to reflux for 2.5 hours. After cooling to room temperature, the reaction mixture was diluted with ethyl ether (60 mL) and cooled in a refrigerator until a white solid precipitated. The solid was filtered through Celite and the filtrate was evaporated in vacuo, affording the title compound as a clear oil (1.85 g, ˜100%). 1H NMR (CDCl3, 500 MHz) δ 4.10 (m, 2H), 3.73 (m, 2H), 1.84 (m, 2H), 1.46 (s, 18H).

1. distillationfreshly distilled from potassium carbonate)
2. temperatureThe reaction mixture was heated
3. temperatureto reflux for 2.5 hours
4. additionthe reaction mixture was diluted with ethyl ether (60 mL)
5. temperaturecooled in a refrigerator until a white solid
6. customprecipitated
7. filtrationThe solid was filtered through Celite
8. customthe filtrate was evaporated in vacuo