HRID745725

反应详情

EQUATION

反应方程式

HRID 745725 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Chloromethanephosphonic acid (4.0 g, 30.6 mmoles) and 1.9-diaminononane (20.1 g, 127.2 mmoles) were dissolved in water (100 cm3) and the resultant solution heated under reflux for 20 hours. The water was then distilled off and methanol (80 cm3) added to the residue. The solid was filtered off, washed with methanol (2×50 cm3) and dried in a vacuum oven at 60° C. for three hours to yield the crude N-(9-aminononyl)aminomethanephosphonic acid monohydrate (6.5 g, 78.5%), having a melting point of 240°-241° C.

WORKUP

后处理

  1. temperatureunder reflux for 20 hours
  2. distillationThe water was then distilled off
  3. additionmethanol (80 cm3) added to the residue
  4. filtrationThe solid was filtered off
  5. washwashed with methanol (2×50 cm3)
  6. customdried in a vacuum oven at 60° C. for three hours