HRID1876332
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 (9 mg, 0.03 mmol) prepared in Example 42 was dissolved in N,N-dimethylformamide (1 ml). Ethylamine hydrochloride (3 mg, 0.03 mmol), EDC (8 mg, 0.04 mmol), HOBT (5 mg, 0.04 mmol) and triethylamine (8 mg, 0.08 mmol) were added thereto, and the mixture was stirred for 8 h at room temperature. After completion of the reaction, saturated sodium bicarbonate solution was added. The mixture was extracted with ethyl acetate, dried over anhydrous magnesium sulfate, and filtered. The filtrate was distilled under reduced pressure, and concentrated. The residue was purified by column chromatography to give the title compound (4 mg, Yield 41%).
WORKUP
后处理
- additionwas added
- extractionThe mixture was extracted with ethyl acetate
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- distillationThe filtrate was distilled under reduced pressure
- concentrationconcentrated
- customThe residue was purified by column chromatography