Reaction #346664

Reaction equation

1,4,7-triazacyclodecane

hexamethylphosphorous triamide

→

1,4,7-triaza-11-phosphatricyclo[5.3.1.04,11 ] undecane

Yield 89.0%

Solvents

toluene

Conditions

Workup

1. 1
   OtherThe toluene is removed under reduced pressure
2. 2
   workup.DISTILLATIONthe residue is distilled through a short-path column

Procedure

A solution of 5.00 g of 1,4,7-triazacyclodecane and 5.70 g of hexamethylphosphorous triamide in 50 ml. of toluene is refluxed for 48 hours. The toluene is removed under reduced pressure, and the residue is distilled through a short-path column, to give 5.31 g (89%) of 1,4,7-triaza-11-phosphatricyclo[5.3.1.04,11 ] undecane as a clear, colorless liquid having a boiling point of 96°-98° C. at 0.70 mm. The product solidifies on standing at room temperature.

Source