反应详情

A solution of 1.75 g of 1,4,7,10-tetraazacyclododecane and 1.63 g of hexamethylphosphorous triamide in 50 ml of toluene is refluxed for 12 hours. Titration of the off-gases with 1 N HCl indicates that 97% of the theoretical amount of dimethylamine is evolved in this time. The toluene is removed under reduced pressure to give 2.0 g of 1,4,7,10-tetraaza-13-phosphatricyclo[5.5.1.04,13 ]tridecane as a white solid which melts at 109°-111° C. with sintering from 90° C. (possibly because of the presence of a trace of toluene). Sublimation of this product at 75° C. and 0.55 mm gives large colorless crystals, which melt at 111°-113° C. The mass spectrum shows an M+ ion at 200; measured mass, 200.1194; calc'd, 200.1190.

1. customThe toluene is removed under reduced pressure