Phosphorus oxychloride → Phosphoramidic dichloride, bis(2-chloroethyl)-
Reaktionsgleichung
Cl.[Cl:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][Cl:8].[P:9](Cl)([Cl:12])([Cl:11])=[O:10]>>[Cl:2][CH2:3][CH2:4][N:5]([CH2:6][CH2:7][Cl:8])[P:9]([Cl:12])([Cl:11])=[O:10]Komponenten
3
Versuchsvorschrift
A suspension of 50 g of bis(2-chloroethyl)amine hydrochloride in 130 mL of distilled phosphorus oxychloride, bp 105.5-107.5° C., was heated under reflux for 12 hours until complete solution resulted. The excess phosphorus oxychloride was removed by distillation and the residue was distilled under reduced pressure. The fraction, bp 123-125°C./0.6 mm Hg, was collected as a water-clear fluid which crystallised as a solid mass on cooling, 58 g, mp 54-56°C. The product crystallised from acetone-petroleum ether, after standing in the cold, in large prisms, mp 54-56° C.
Aufarbeitung
- temperaturewas heated
- temperatureunder reflux for 12 hours until complete solution
- customresulted