HRID2258393

反应详情

EQUATION

反应方程式

HRID 2258393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 143.9 g of 1,4,7,10-tetraazacyclododecane (product commercially available) (0.84 mol) in 1000 ml of CH3CN under reflux, a suspension of 50 g of compound (A) 3-[(2-chloro-1-oxoethyl)amino]-2,4,6-triiodobenzoic acid (0.084 mol) in 500 ml of CH3CN is added during 1 h. The mixture is kept under reflux for 24 h, yielding a solid precipitation. The reaction mixture is filtered and the solid is purified by chromatography on silica gel. 55 g of N-(3-carboxy-2,4,6-triiodophenyl)-1,4,7,10-tetraazacyclododecane-1-acetamide (0.076 mol) are obtained.

WORKUP

后处理

  1. additionis added during 1 h
  2. temperatureunder reflux for 24 h
  3. customyielding
  4. customa solid precipitation
  5. filtrationThe reaction mixture is filtered
  6. customthe solid is purified by chromatography on silica gel