反应详情

温度

-78 °C

Tertiary-butyl(diethoxymethyl)phosphine oxide (2.5 g), (0.012 mol) is dissolved in 35 ml of dry tetrahydrofuran and cooled to -78° C. under an argon atmosphere. To this stirred solution is added 9.0 ml of n-butyl lithium (1.6M solution in hexane) and the mixture is stirred at -78° C. for 10 minutes. After this time, a solution of 2.47 g (0.014 mol) of benzyl bromide in 15 ml of dry tetrahydrofuran is added, and the reaction mixture is allowed to warm to room temperature. After stirring for 3 hours at room temperature, 10 ml of saturated ammonium chloride solution is added and the product is extracted into diethyl ether (2×100 ml). The combined organic extracts are dried and evaporated under reduced pressure to give a crude product. This is purified by chromatography on silica, using ethyl acetate as eluent, to give tertiary-butyl(benzyl)(diethoxymethyl) phosphine oxide as a colourless oil.

1. temperatureto warm to room temperature
2. stirringAfter stirring for 3 hours at room temperature
3. extractionthe product is extracted into diethyl ether (2×100 ml)
4. customThe combined organic extracts are dried
5. customevaporated under reduced pressure
6. customto give a crude product
7. customThis is purified by chromatography on silica