HRID1418270

反应详情

EQUATION

反应方程式

HRID 1418270 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N,N'-Bis(2,2-dimethyl-1,3-dioxolane-4-carbonyl)-3,5-diamino-2,4,6-triiodobenzylacetate (1.25 g, 1.55 mol) was dissolved in a mixture of water (50 ml), methanol (25 ml) and concentrated HCl (0.5 ml). After stirring for 4 h, the solution was neutralized with aqueous NaH2PO4 and the solvents were removed by evaporation. The residue was dissolved in water (10 ml) and the pH was adjusted to 12 with aqueous NaOH. After 30 min, the solution was again neutralized and the solvent was evaporated. The product was purified by preparative HPLC. Yield: 483 mg (45%).

WORKUP

后处理

  1. customthe solvents were removed by evaporation
  2. dissolutionThe residue was dissolved in water (10 ml)
  3. waitAfter 30 min
  4. customthe solvent was evaporated
  5. customThe product was purified by preparative HPLC