Reaction #346665

Reaction equation

1,5,9-triazacyclododecane

hexamethylphosphorous triamide

dimethylamine

→

1,5,9-triaza- 13-phosphatricyclo[7.3.1.05,13 ]tridecane

Yield 76.0%

Conditions

Workup

1. 1
   workup.DISTILLATIONDistillation under reduced pressure

Procedure

A mixture of 4.20 g of 1,5,9-triazacyclododecane and 4.00 g of hexamethylphosphorous triamide is heated at 100° C. for about 6 hours, by which time evolution of dimethylamine is complete. Distillation under reduced pressure gives 3.70 g (76%) of 1,5,9-triaza- 13-phosphatricyclo[7.3.1.05,13 ]tridecane as a clear, colorless liquid which boils at 104°-135° C. at 0.60 mm. The product solidifies at room temperature. Its infrared absorption spectrum (neat) shows absorptions at 3.5, 6.85, 7.01, 7.52, 7.73, 8.00, 8.27, 8.66, 8.90, 9.02, 9.36, 9.56, 10.27, 10.89, 11.42, 11.73, 11.97 and 14.7 μ. The mass spectrum shows an M+ ion at 199; measured mass, 199.1264; calc'd, 199.1238.

Source