Diisopropylamine → HCID 86744989, compound

Participants

Reaction Steps

127 g (0.96 mol) of phosphorous acid methyl ester-dichloride are initially taken in a mixture of 250 ml of absolute ether and 250 ml of absolute pentane, and a solution of 270 ml (1.92 mol) of diisopropylamine in 100 ml of absolute ether and 100 ml of absolute pentane is added dropwise in the course of 2 hours at -15° C., with vigorous stirring and nitrogen blanketing. The reaction mixture is allowed to heat up to room temperature while being stirred, and is then stirred for a further 2 hours. It is then cooled to -15° C. again, and the hydrochloride is removed from the reaction solution by filtration under an inert gas. The filter cake is rinsed with 750 ml of a cold mixture of equal volumes of absolute ether and absolute pentane. The filtrates are combined, and the solvents are removed under a water pump vacuum. The residue is subjected twice to a high-vacuum distillation through an 80 cm Vigreux column. This gives 80 g of a main fraction (boiling point 38 to 41° C. at 0.1 mbar) which, according to 31P-NMR, is composed of 99% of a single substance (δ=185 ppm).

Provenance & Evidence