反应 #985248

反应方程式

pyridine

PCl3

AlCl3

fluorobenzene

→

p-fluorophenyldichlorophosphine

收率 47.0%

反应条件

后处理

1. 1
   其他A 1 l flask equipped with a thermostated jacket, mechanical stirring
2. 2
   温度thermometer and reflux condenser
3. 3
   其他mist formed
4. 4
   workup.STIRRINGStirring
5. 5
   workup.WAITwas then continued at 60° C. for a further 30 min
6. 6
   其他An irregular, large-lumped solid precipitated which could not
7. 7
   其他be removed via a suction
8. 8
   过滤filter
9. 9
   过滤only by filtration
10. 10
    过滤The residue which was filtered off
11. 11
    洗涤was washed with petroleum ether
12. 12
    洗涤The filtrate and washing liquid
13. 13
    workup.DISTILLATIONdistilled

实验过程

A 1 l flask equipped with a thermostated jacket, mechanical stirring, thermometer and reflux condenser was initially charged under an argon atmosphere with a mixture of 3.4 mol of PCl3 and 1.2 mol of AlCl3 (98% purity) at 73° C. 0.8 mol of fluorobenzene was then added within 30 min, while a weak argon stream was passed through the reaction flask. The reaction mixture was stirred for 3 hours and cooled to 60° C., and 1.25 mol of pyridine were added slowly within 45 min. The reaction was exothermic and mist formed. Stirring was then continued at 60° C. for a further 30 min. An irregular, large-lumped solid precipitated which could not be removed via a suction filter, but only by filtration. The residue which was filtered off was washed with petroleum ether. The filtrate and washing liquid were combined and distilled to obtain 73.3 g of p-fluorophenyldichlorophosphine in a yield of 47% of theory.

来源