反应详情

温度

170 °C

Triisopropyl phosphite (0.33 ml, 1.2 mmol) was added to the 2-phosphono-5-bromotetrahydrofuran prepared in accordance with the process of Example II. The mixture was heated over a period of one half hour under a nitrogen atmosphere to 170° C. It was held at this temperature for two and one quarter hours and then cooled to room temperature. Concentrated hydrochloric acid (15 ml) was added and the resulting mixture was heated to reflux for five hours. The volatile components were removed under vacuum leaving 2,5-diphosphonotetrahydrofuran ("DPTHF") containing phosphorous acid as an impurity. The identity of the 2,5-diphosphonotetrahydrofuran was established by nuclear magnetic resonance spectroscopy (proton, phosphorus and carbon-13) and fast atom bombardment mass spectroscopy

1. customprepared in accordance with the process of Example II
2. waitIt was held at this temperature for two and one quarter hours
3. temperaturecooled to room temperature
4. temperaturethe resulting mixture was heated
5. temperatureto reflux for five hours
6. customThe volatile components were removed under vacuum