反应详情

A solution of 2.50 g of 1-oxa-4,7,10-triazacyclododecane and 2.35 g of hexamethylphosphorous triamide in 25 ml of toluene is refluxed for forty hours. It is then concentrated to dryness in a rotary evaporator, to give 2.97 g (100%) of 10-oxa-1,4,7-triaza-13-phosphatricyclo[5.5.1.04,13 ]tridecane as a brittle, white solid. Sublimation at 80° C (0.007 mm) gives 2.08 g of white crystals having a melting point of 68°-70° C.

1. concentrationIt is then concentrated to dryness in a rotary evaporator