HRID1065064

反应详情

EQUATION

反应方程式

HRID 1065064 的结构方程式

PROCEDURE

实验过程

6.6 g of 5-cyano-3-[N-(2,3-dihydroxypropyl)carbamoyl]-2,4,6-triiodobenzoic acid chloride is dissolved in 40 ml of dimethylacetamide and combined with 2.3 g of N-methylamino-2,3-propanediol. The mixture is stirred for one hour at room temperature and then concentrated under vacuum. The thus-obtained crude product can be used directly for nitrile saponification. To isolate the pure product the dilute aqueous solution of the crude product is treated with a cation exchange resin and an anion exchange resin, and the filtered solution is concentrated under vacuum to dryness, thus obtaining 5.9 g (81% of theory) of 3-[N-(2,3-dihydroxypropyl)carbamoyl]-5-[N-(2,3-dihydroxypropyl)-N-methylcarbamoyl]-2,4,6-triiodobenzonitrile; mp 215° C.

WORKUP

后处理

  1. concentrationconcentrated under vacuum
  2. customThe thus-obtained crude product
  3. customTo isolate the pure product the dilute aqueous solution of the crude product
  4. additionis treated with a cation exchange resin
  5. concentrationan anion exchange resin, and the filtered solution is concentrated under vacuum to dryness