Reaktion #346664

ord-3d1a6ff81f5d47468adb9d1add2ab010

Reaktionsgleichung

C1CNCCNCCNC1
1,4,7-triazacyclodecane
CN(C)P(N(C)C)N(C)C
hexamethylphosphorous triamide
C1CN2CCN3CCN(C1)P23
1,4,7-triaza-11-phosphatricyclo[5.3.1.04,11 ] undecane
Ausbeute 89.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe toluene is removed under reduced pressure
  2. 2
    workup.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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04038312uspto-grants-1977_07