Triethylamine → Bis-pyrrolidinochlorophosphine oxide

Participants

Reaction Steps

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##

Provenance & Evidence