HRID348670

反应详情

EQUATION

反应方程式

HRID 348670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The compound (0.78 g) obtained in Example 25-4 was dissolved in methanol (20 ml) and added with 2-imidazole carboxaldehyde (214.6 mg), followed by stirring at room temperature for 17 hours. After the solvent had been distilled off, the residue was dried under vacuum and then dissolved in methanol (15 ml) and then added with sodium borohydride (217.8 mg), followed by stirring at room temperature for 45 minutes. The reaction solution was added with a saturated aqueous ammonium chloride solution (10 ml) and stirred at room temperature for 15 minutes. Then, the reaction solution was added with saturated saline solution and extracted with chloroform, followed by drying with anhydrous sodium sulfate. After the solvent had been distilled off, the residue obtained was purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (1.01 g) as a yellow solid.

WORKUP

后处理

  1. distillationAfter the solvent had been distilled off
  2. customthe residue was dried under vacuum
  3. dissolutiondissolved in methanol (15 ml)
  4. additionadded with sodium borohydride (217.8 mg)
  5. stirringby stirring at room temperature for 45 minutes
  6. additionThe reaction solution was added with a saturated aqueous ammonium chloride solution (10 ml)
  7. stirringstirred at room temperature for 15 minutes
  8. additionThen, the reaction solution was added with saturated saline solution
  9. extractionextracted with chloroform
  10. dry with materialby drying with anhydrous sodium sulfate
  11. distillationAfter the solvent had been distilled off
  12. customthe residue obtained
  13. customwas purified through silica gel column chromatography (chloroform/ethyl acetate)