反应详情

A stirred mixture of 4.90 g (30 mmol) of hexamethylphosphorous triamide, 6.00 g (30 mmol) of 1,4,8,11-tetraazacyclotetradecane, and 30 ml of dry toluene is heated to 80°-90°, under nitrogen for 16 hr, then refluxed for 8 hr. The hot solution is filtered under N2 and concentrated, and the residue is sublimed at 60°-70° (0.3 mm) to give 5.45 g (80%) of waxy, white solid 1,4,8,11-tetraaza-15-phosphatetracyclo[6.6.1.04,15.011,15 ]pentadecane.

1. temperatureis heated to 80°-90°, under nitrogen for 16 hr
2. temperaturerefluxed for 8 hr
3. filtrationThe hot solution is filtered under N2
4. concentrationconcentrated
5. customis sublimed at 60°-70°