HRID493388

反应详情

EQUATION

反应方程式

HRID 493388 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-{4-[2-(phenoxymethyl)-1H-imidazol-4-yl]phenoxy}aniline (238 mg, 0.0066 mol), (prepared according to a method analogous to that described in Example 28) is suspended in dichloromethane (5 ml) at 23° C. Triethylamine (0.1 ml, 0.0079 mol) and acetic anhydride (0.062 ml, 0.0066 mol) are added. The mixture is then stirred for 20 hours then evaporated to dryness. The oil obtained is taken up with ethyl acetate and water. After decantation and extraction by ethyl acetate, the organic phase is washed with water then with a saturated solution of sodium chloride, dried over sodium sulphate then the solvent is evaporated off. The residue obtained is adsorbed on silica then purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 7-3 to 9-1). After washing with diisopropyl ether and isopentane, a beige-coloured powder is obtained.

WORKUP

后处理

  1. customthen evaporated to dryness
  2. customThe oil obtained
  3. extractionAfter decantation and extraction by ethyl acetate
  4. washthe organic phase is washed with water
  5. dry with materialwith a saturated solution of sodium chloride, dried over sodium sulphate
  6. customthe solvent is evaporated off
  7. customThe residue obtained
  8. customthen purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 7-3 to 9-1)
  9. washAfter washing with diisopropyl ether and isopentane
  10. customa beige-coloured powder is obtained