HRID745720

反应详情

EQUATION

反应方程式

HRID 745720 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Chloromethanephosphonic acid (6.5 g, 49.8 mmoles) and 1.6-diaminohexane (34.8 g, 300 mmoles) were dissolved in water (130 cm3) and heated under reflux for 20 hours. The water was removed and ethanol (250 cm3) was added to the solid residue. The phosphonic acid was filtered off and dried. The crude yield was 10.4 g (92%). A sample was purified by recrystallization from water/ethanol to give N-(6-aminohexyl)-aminomethanephosphonic acid monohydrate as a fine white crystalline solid having a melting point of 235° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 20 hours
  3. customThe water was removed
  4. additionethanol (250 cm3) was added to the solid residue
  5. filtrationThe phosphonic acid was filtered off
  6. customdried
  7. customA sample was purified by recrystallization from water/ethanol