HRID1065063

反应详情

EQUATION

反应方程式

HRID 1065063 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

18.1 g of 5-cyano-2,4,6-triiodoisophthalic acid dichloride is combined in 750 ml of dioxane at 80° C. with 7.1 g of 1-amino-2,3-propanediol and stirred for 2 hours. The mixture is then separated from the precipitated hydrochloride of 1-amino-2,3-propanediol, and the filtrate is concentrated under vacuum. The residue is extracted by boiling with 800 ml of ethyl acetate. After concentration and cooling, 11.7 g (59% of theory) of 5-cyano-3-[N-(2,3-dihydroxypropyl)carbamoyl]-2,4,6-triiodobenzoyl chloride is crystallized from the extract as a white powder; mp 285°-288° C.

WORKUP

后处理

  1. customThe mixture is then separated from the precipitated hydrochloride of 1-amino-2,3-propanediol
  2. concentrationthe filtrate is concentrated under vacuum
  3. extractionThe residue is extracted
  4. concentrationAfter concentration
  5. temperaturecooling
  6. custom11.7 g (59% of theory) of 5-cyano-3-[N-(2,3-dihydroxypropyl)carbamoyl]-2,4,6-triiodobenzoyl chloride is crystallized from the
  7. extractionextract as a white powder