Reaktion #346663

Reaktionsgleichung

1-oxa-4,7,10-triazacyclododecane

hexamethylphosphorous triamide

→

10-oxa-1,4,7-triaza-13-phosphatricyclo[5.5.1.04,13 ]tridecane

Ausbeute 102.5%

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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 40 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.

Quelle