HRID52764
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
Bis(3,5-difluorophenyl)phosphinous acid (4.78 g=0.0174 mole) was placed in a 50 mL round bottom flask equipped with a magnetic stirring bar and a condenser with a nitrogen inlet tube. To this was added phenylsilane (1.54 g=0.014 mole). With stirring, the reaction was heated to 130° C. for three hours. As the temperature rose, the mixture became homogeneous and remained as such. After three hours, the reaction mixture was distilled, collecting the fraction boiling at 128°-138° C. at 0.05 mm Hg. The yield of bis(3,5-difluorophenyl)phosphine was 2.45 g (54%). The 3P absorption is at -37 ppm (relative to external H3PO4).
WORKUP
后处理
- customequipped with a magnetic stirring bar and a condenser with a nitrogen inlet tube
- distillationthe reaction mixture was distilled
- customcollecting the fraction boiling at 128°-138° C. at 0.05 mm Hg
- customThe 3P absorption