HRID1065063
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe mixture is then separated from the precipitated hydrochloride of 1-amino-2,3-propanediol
- concentrationthe filtrate is concentrated under vacuum
- extractionThe residue is extracted
- concentrationAfter concentration
- temperaturecooling
- custom11.7 g (59% of theory) of 5-cyano-3-[N-(2,3-dihydroxypropyl)carbamoyl]-2,4,6-triiodobenzoyl chloride is crystallized from the
- extractionextract as a white powder