反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- distillationAfter the solvent had been distilled off
- customthe residue was dried under vacuum
- dissolutiondissolved in methanol (15 ml)
- additionadded with sodium borohydride (217.8 mg)
- stirringby stirring at room temperature for 45 minutes
- additionThe reaction solution was added with a saturated aqueous ammonium chloride solution (10 ml)
- stirringstirred at room temperature for 15 minutes
- additionThen, the reaction solution was added with saturated saline solution
- extractionextracted with chloroform
- dry with materialby drying with anhydrous sodium sulfate
- distillationAfter the solvent had been distilled off
- customthe residue obtained
- customwas purified through silica gel column chromatography (chloroform/ethyl acetate)