At 0 °C, a solution of 27.0 g (97.6 mmol) of ST913 in 100 mL of anhydrous tetrahydrofuran was added together with a solution of 44.4 mL (97.6 mmol) of 2,2 N-butyllithium in hexane. After stirring at room temperature for 1 hour, the reaction mixture was evaporated, and the residue was dissolved in toluene petroleum ether. The precipitated lithium chloride was filtered off, and the res solution was evaporated. The residue was purified by short-path distillation under high vacuum (220–230 °C/0.1 mbar). 15.3 g of cyanomethylenetri-n-butylphosphine (65% of the theoretical value) was given as a colorless liquid.
Figure: Synthetic Route of CYANOMETHYLENETRIBUTYLPHOSPHORANE
