Реакция #76362

Уравнение реакции

bis(2-chloroethyl)amine hydrochloride

phosphorus oxychloride

→

N,N-Bis(2-chloroethyl)phosphoramidic dichloride

Условия реакции

Обработка

1. 1
   Температураwas heated
2. 2
   Температураunder reflux for 12 hours until complete solution
3. 3
   Другоеresulted
4. 4
   ДругоеThe excess phosphorus oxychloride was removed by distillation
5. 5
   workup.DISTILLATIONthe residue was distilled under reduced pressure
6. 6
   ДругоеThe fraction, bp 123-125°C./0.6 mm Hg, was collected as a water-clear fluid which
7. 7
   Другоеcrystallised as a solid mass
8. 8
   Температураon cooling
9. 9
   ДругоеThe product crystallised from acetone-petroleum ether

Методика

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.

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