反应详情

To a mixture of 0.26 g (0.011 mol) of sodium metal in 35 ml of dry THF was added 3.14 g (0.023 mol) of diethyl phosphite. This solution was stirred at room temperature under a N2 atmosphere for 18 hours. To this salt solution was added 2.0 g (0.006 mol) of product of Example 107. This mixture was stirred at reflux for 18 hours. The mixture was cooled to room temperature and poured into H2O. The H2O mixture was extracted twice with diethyl ether. The combined ether phases were then washed with H2O, dried (MgSO4), and concentrated in vacuo affording 2.18 g of an orange oil. This oil was kugelrohr distilled at 80 and collected at 150°-151° C. pot temperature yielding 1.68 g (63%) of a clear oil, n25D 1.4536.

1. stirringThis mixture was stirred
2. temperatureat reflux for 18 hours
3. temperatureThe mixture was cooled to room temperature
4. extractionThe H2O mixture was extracted twice with diethyl ether
5. washThe combined ether phases were then washed with H2O
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo