HRID476849

反应详情

EQUATION

反应方程式

HRID 476849 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

A solution containing 0.025 moles of P,P-bis(2,2-dimethyl-1-aziridinyl)phosphinyl chloride in about 170 milliliters of THF was prepared in accordance with Example 1, chilled to -40° C. and treated, by slow dropwise addition, with a solution containing 0.026 moles of 3-dimethylaminopropylamine, in 25 milliliters of THF. The resulting slurry was stirred overnight at ambient temperature, filtered, the filtrate was concentrated by rotary evaporation, and vacuum distilled at 119° C./0.45 millimeter of mercury to produce a 40% yield of P,P-bis(2,2-dimethyl-1-aziridinyl)-N-(3-dimethylaminopropyl)phosphinic amide. NMR characterization confirmed the product was 99% pure. Elemental analysis confirmed the structure contained the following:

WORKUP

后处理

  1. customwas prepared in accordance with Example 1
  2. additiontreated, by slow dropwise addition, with a solution
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated by rotary evaporation, and vacuum
  5. distillationdistilled at 119° C./0.45 millimeter of mercury