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 (817.3 mg) obtained in Example 102-2 was dissolved in anhydrous methanol (24.5 ml) and added with 1-methyl-2-imidazolealdehyde (309.4 mg) and sodium cyanoborohydride (235.0 mg). Then, the solution was adjusted to pH 5 with acetic acid and stirred at room temperature for 24 hours. After the reaction, the solvent was distilled off. The residue was added with a 1 mol/l sodium hydroxide aqueous solution and then subjected to extraction with chloroform. The extract was dried with anhydrous magnesium sulfate and the solvent was distilled off. Subsequently, the residue was purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (910.0 mg) as a white solid.
WORKUP
后处理
- customAfter the reaction
- distillationthe solvent was distilled off
- additionThe residue was added with a 1 mol/l sodium hydroxide aqueous solution
- extractionsubjected to extraction with chloroform
- dry with materialThe extract was dried with anhydrous magnesium sulfate
- distillationthe solvent was distilled off
- customSubsequently, the residue was purified through silica gel column chromatography (chloroform/methanol)