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 (57.2 mg) obtained in Example 19-2, the compound (106 mg) obtained in Example 2-2, and HOBt (162 mg) were dissolved in anhydrous DMF (2.5 ml) and then added with PS-carbodiimide (manufactured by Argonaut Technologies, Inc.) (419 mg), followed by stirring at room temperature for 12 hours. After completion of the reaction, the solution was filtrated and the solvent was then distilled off. The residue was dissolved in chloroform and then washed with 1 mol/l sodium hydroxide and saturated saline solution, followed by drying with anhydrous magnesium sulfate. The solvent was distilled off and the residue was then treated with hydrochloric acid. Subsequently, the residue was purified through silica gel column chromatography (chloroform/methanol/water), thereby obtaining hydrochloride (18.3 mg) of the subject compound as a yellow solid.
WORKUP
后处理
- customAfter completion of the reaction
- filtrationthe solution was filtrated
- distillationthe solvent was then distilled off
- dissolutionThe residue was dissolved in chloroform
- washwashed with 1 mol/l sodium hydroxide and saturated saline solution
- dry with materialby drying with anhydrous magnesium sulfate
- distillationThe solvent was distilled off
- additionthe residue was then treated with hydrochloric acid
- customSubsequently, the residue was purified through silica gel column chromatography (chloroform/methanol/water)