反应详情

The bis-pyrrolidinochlorophosphine oxide was prepared as follows: 56.8 g (0.8 mole) pyrrolidine, 80.8 g (0.8 mole) triethylamine and 300 ml dry benzene were charged into a 1 liter three-necked flask equipped with a stirrer, condenser and dropping funnel. A solution of POCl3 in 70 mls dry benzene was added dropwise under a stream of dry nitrogen. The reaction was exothermic. On complete addition of the POCl3 /benzene solution, the reaction mixture was stirred for 11/2 hours at room temperature. The precipitated triethylamine hydrochloride was filtered off and the filtrate evaporated using a rotary evaporator under reduced pressure (60 mm). The product was fractionally distilled under reduced pressure (0.3 - 0.5 mm) and the fraction distilling between 138°-140° collected. This fraction was identified as ##EQU59##

1. customequipped with a stirrer, condenser
2. filtrationThe precipitated triethylamine hydrochloride was filtered off
3. customthe filtrate evaporated
4. customa rotary evaporator under reduced pressure (60 mm)
5. distillationThe product was fractionally distilled under reduced pressure (0.3 - 0.5 mm)
6. distillationthe fraction distilling between 138°-140°
7. customcollected