HRID1604157

反应详情

EQUATION

反应方程式

HRID 1604157 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3-Hydroxymethyl-5-(2,3-dihydroxypropylaminocarbonyl)-2,4,6-triiodoaniline (1.89 g, 3.06 mmol) prepared according to Example 3d, was dissolved in a mixture of acetic anhydride (5 ml) and pyridine (5 ml). The mixture was stirred at room temperature for 24 h, CH2Cl2 (100 ml) was added and the solution was washed with water (3×25 ml), with a saturated aqueous solution of NaHCO3, dried (Na2SO4) and evaporated. The product was purified by flash chromatography on silica gel using a mixture of CH2Cl2 and methanol (98:2) as the eluent. Yield: 1.30 g (57%).

WORKUP

后处理

  1. washthe solution was washed with water (3×25 ml), with a saturated aqueous solution of NaHCO3
  2. dry with materialdried (Na2SO4)
  3. customevaporated
  4. customThe product was purified by flash chromatography on silica gel using
  5. additiona mixture of CH2Cl2 and methanol (98:2) as the eluent