反应详情

温度

70 °C

A 37% of formaldehyde solution, 16.2 g, was added in small portions over a five minute period to solution of 40 ml of methanol, 21.78 g of di-n-propyl phosphine oxide, (Example 16), and 1.5 ml of triethylamine. The reaction exothermed to 30° C. and was allowed to stir for ten minutes before it was warmed to 70° C. for three hours. The reaction was then allowed to cool to room temperature and stand overnight. The reaction was concentrated, the concentrate dissolved in 70 ml of THF, filtered and reconcentrated. The concentrate was diluted with 60 ml of 1,4-dioxane which was distilled off to yield 19.8 g of the desired phosphine oxide as an oil.

1. customexothermed to 30° C.
2. temperatureto cool to room temperature
3. concentrationThe reaction was concentrated
4. dissolutionthe concentrate dissolved in 70 ml of THF
5. filtrationfiltered
6. additionThe concentrate was diluted with 60 ml of 1,4-dioxane which
7. distillationwas distilled off