Reaktion #346664
ord-3d1a6ff81f5d47468adb9d1add2ab010
Reaktionsgleichung
1,4,7-triazacyclodecane
hexamethylphosphorous triamide
→
1,4,7-triaza-11-phosphatricyclo[5.3.1.04,11 ] undecane
Ausbeute 89.0%
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe toluene is removed under reduced pressure
- 2workup.DISTILLATIONthe residue is distilled through a short-path column
Vorschrift
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.