Phosphorus oxychloride → Phosphoramidic dichloride, bis(2-chloroethyl)-

Participants

Reaction Steps

A mixture of bis(2-chloroethyl)amine hydrochloride (5 g) and POCl3 (13 mL) was heated at reflux for 12 hours, during which the mixture became a homogeneous solution. The excess POCl3 was removed by distillation (bp 105° C.), and then 4.93 g of the product was distilled (bp 110-114° C., 0.1 mm Hg). Recrystalliztion from acetone/hexane gave 4.5 g of the product as a colorless solid: mp 54.5-56° C. (lit. 54-56° C., Friedman, O. M., et. al., J. Am. Chem. Soc. 76 (1954):655-658); 1H NMR (CDCl3) δ 3.62-3.68 (m, 2), 3.71-3.77 (m, 6).

Provenance & Evidence