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 (73 mg, 0.157 mmol) obtained in Example 1k was dissolved in methylene chloride (3 mL), 5-formyl-thiophene-2-carboxylic acid (40 mg, 0.257 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (89 mg, 0.464 mmol) were added, and the mixture was stirred at room temperature for 1.5 hours. A saturated aqueous sodium hydrogencarbonate solution was added, and then the mixture was extracted with ethyl acetate (×3) and dried with anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (methylene chloride:methanol=40:1→20:1, v/v) to give the title compound (144 mg; yield, 61%) as a white solid.
WORKUP
后处理
- extractionthe mixture was extracted with ethyl acetate (×3)
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe resulting residue was purified by silica gel column chromatography (methylene chloride:methanol=40:1→20:1, v/v)