HRID2249139
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
137 g of 5-amino-2,4,6-triiodoisophthaloyl chloride (0.23 mole) are dissolved in 460 ml of DMAC to which are added 110 g (0.57 mole) of 2-isopropyl-1,3-dioxane-5-carboxylic acid chloride. The reaction mixture is stirred under argon at ambient temperature for 4 days. The DMAC is removed in a vacuum. The oil obtained is extracted with 3 l of ethyl acetate and washed twice with 1 l of ice-cold water. The organic phase is dried and concentrated to dryness. The product is crystallized from 200 ml of CH2Cl2. After filtration, 110 g of solid are obtained:
WORKUP
后处理
- customThe DMAC is removed in a vacuum
- customThe oil obtained
- extractionis extracted with 3 l of ethyl acetate
- washwashed twice with 1 l of ice-cold water
- customThe organic phase is dried
- concentrationconcentrated to dryness
- customThe product is crystallized from 200 ml of CH2Cl2
- filtrationAfter filtration, 110 g of solid
- customare obtained