反应详情

温度

-70 °C

30 g (0.097 mol) of diethyl 5-(tetrahydropyran-2-yloxy)pentylphosphonate were initially introduced into 200 ml of absolute tetrahydrofuran under an argon atmosphere, cooled to -70° C. and treated with 42.8 ml (0.107 mol) of a 2.5 molar solution of butyllithium in hexane. After addition, the solution was stirred for a further 30 minutes and 15.6 g (0.11 mol) of methyl iodide were then slowly added dropwise. The mixture was stirred at -70° C. for a further 2 hours and at room temperature for 4 hours, cautiously treated with a saturated sodium chloride solution and taken up in ethyl acetate. The organic phase was washed with water and a saturated sodium chloride solution, dried over sodium sulfate and distilled in a bulb tube.

1. additionAfter addition
2. stirringThe mixture was stirred at -70° C. for a further 2 hours and at room temperature for 4 hours
3. washThe organic phase was washed with water
4. dry with materiala saturated sodium chloride solution, dried over sodium sulfate
5. distillationdistilled in a bulb tube