Phosphorus oxychloride → Phosphoramidic dichloride, bis(2-chloroethyl)-

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.

1. temperaturewas heated
2. temperatureunder reflux for 12 hours until complete solution
3. customresulted
4. customThe excess phosphorus oxychloride was removed by distillation
5. distillationthe residue was distilled under reduced pressure
6. customThe fraction, bp 123-125°C./0.6 mm Hg, was collected as a water-clear fluid which
7. customcrystallised as a solid mass
8. temperatureon cooling
9. customThe product crystallised from acetone-petroleum ether

ORDレコード

ord-fb68e373267a4e068460ead9ebad4ac5

出典データセット

uspto-grants-2004_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06702705B1