Phosphine, dibutyl(1,1-dimethylethyl)- synthesis

Yield:29949-71-1 56%

Reaction Conditions:

in diethyl ether;hexane at -20 - 20;Heating / reflux;

Steps:

tert.-Butyl-di-n-butylphosphine (^tBuPⁿBu₂); 10.3 g (65 mmol) of tert-butyldichlorophosphine (from Aldrich, 82018 Taufkirchen, Germany) were introduced under nitrogen in a 100 ml round-bottom flask at room temperature, dissolved in 20 ml of diethyl ether and cooled while stirring to -20° C. 55 ml of a 2.5 M solution of n-butyllithium in n-hexane (from Aldrich) were subsequently added dropwise, resulting in a white solid precipitating immediately with considerable evolution of heat. After the addition was complete, the mixture was warmed slowly to room temperature, subsequently refluxed for one hour, cooled to room temperature and admixed with 10 ml of 10% strength, oxygen-free, aqueous HCl, resulting in two clear, colourless phases being formed. After phase separation, the organic phase was freed of the major part of the solvent by distillation under atmospheric pressure, subsequently filtered and the filtrate was distilled under reduced pressure. This gave 7.4 g (56% of theory) of ^tBuPⁿBu₂, b.p.: 75° C. at 0.2 mbar.

References:

US2008/262262,2008,A1 Location in patent:Page/Page column 4