HRID1462885

反应详情

EQUATION

反应方程式

HRID 1462885 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1000 g of 1,3,5-tricyanobenzene (MTN) was charged in an autoclave having a 20 l capacity together with 400 g of Raney nickel-chromium catalyst (atomic ratio Ni:Cr=49:1), 1800 ml of methanol, 4.2 l of m-xylene and 32.6 g of sodium hydroxide. Hydrogen was injected thereinto under an initial pressure of 140 kg/cm2G and reaction was effected at 60°-102° C. to cause absorption of nearly theoretical amount of hydrogen for 31 minutes. The catalyst was filtered off and the solvent was distilled out. Then, distillation under reduced pressure was effected to obtain 874 g of colorless crystal of 1,3,5-tris(aminomethyl)benzene (MTA). The product had a melting point of 49°-51° C. and a boiling point of 136°-139° C./0.4 mmHg.

WORKUP

后处理

  1. customunder an initial pressure of 140 kg/cm2G and reaction
  2. customwas effected at 60°-102° C.
  3. customabsorption of nearly theoretical amount of hydrogen for 31 minutes
  4. filtrationThe catalyst was filtered off
  5. distillationthe solvent was distilled out
  6. distillationThen, distillation under reduced pressure