HRID477756

反应详情

EQUATION

反应方程式

HRID 477756 的结构方程式

CONDITIONS

反应条件

温度
600 °C

PROCEDURE

实验过程

100 g (=0.513 mol) of phenylphosphonyl dichloride and 200 g (=1.45 mol) of phosphorus trichloride were mixed. This mixture was introduced dropwise, over the course of 3 hours, into a vertical quartz tube which was 60 cm long, filled with 6 mm diameter quartz Raschig rings, was flushed with nitrogen and was located in an electric oven heated to 600° C. The reaction mixture collecting in the trap was again introduced dropwise, over the course of 2 hours, into the quartz tube at 600° C. The reaction mixture now produced was distilled in vacuo. Apart from unreacted phosphorus trichloride and phosphorus oxychloride, 80 g of a distillate were obtained which, on the basis of a 31P NMR spectrum, had the following composition:

WORKUP

后处理

  1. additionThis mixture was introduced dropwise, over the course of 3 hours, into a vertical quartz tube which
  2. customwas flushed with nitrogen
  3. customwas located in an electric oven
  4. customThe reaction mixture collecting in the trap
  5. additionwas again introduced dropwise, over the course of 2 hours, into the quartz tube at 600° C
  6. customThe reaction mixture now produced
  7. distillationwas distilled in vacuo