Reaktion #346666

ord-62cbd32228084c43a59b90ff237f1eb0

Reaktionsbedingungen

Temperatur
125°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeis vigorous for the first 45 minutes
  2. 2
    workup.DISTILLATIONDistillation

Vorschrift

A mixture of 3.62 g of 1,4,8-triazacycloundecane and 3.75 g of hexamethylphosphorous triamide is heated to 125° C. with stirring and held at this temperature for 2 hours, by which time evolution of dimethylamine is complete. Evolution is vigorous for the first 45 minutes. Distillation affords 3.20 g (75%) 1,4,8-triaza-12-phosphatricyclo[6.3.1.04,12 ]dodecane as a water-white liquid which boils at 73°-75° C. at 0.30 mm.

Quelle

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