HRID2249139

反应详情

EQUATION

反应方程式

HRID 2249139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe DMAC is removed in a vacuum
  2. customThe oil obtained
  3. extractionis extracted with 3 l of ethyl acetate
  4. washwashed twice with 1 l of ice-cold water
  5. customThe organic phase is dried
  6. concentrationconcentrated to dryness
  7. customThe product is crystallized from 200 ml of CH2Cl2
  8. filtrationAfter filtration, 110 g of solid
  9. customare obtained