反応 #76362

反応方程式

bis(2-chloroethyl)amine hydrochloride

phosphorus oxychloride

→

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

反応条件

後処理

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

実験手順

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.

出典