HRID1048832

反应详情

EQUATION

反应方程式

HRID 1048832 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

N,N′-Bis-(2-hydroxy-1-hydroxymethyl-ethyl)-5-nitro-isophthalamide (40 g) is dissolved in water (600 mL), and then heated to 90° C. to dissolve. Raney Ni (5 g) is added, and allowed to react for 10 h under a H2 pressure of 1.5 MPa. Raney Ni is removed by filtration and the filter cake washed with 20-30 mL of water. The filtrate and washings are combined to obtain the aqueous solution of 5-Amino-N,N′-bis-(2-hydroxy-1-hydroxymethyl-ethyl)-isophthalamide, which can be utilized directly in the iodination reaction or concentrated and then re-crystallized using methanol to obtain solid product.

WORKUP

后处理

  1. dissolutionto dissolve
  2. customto react for 10 h under a H2 pressure of 1.5 MPa
  3. customRaney Ni is removed by filtration
  4. washthe filter cake washed with 20-30 mL of water