HRID1369067
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
A mixture of 4-pentynoic acid (210 mg, 2.14 mmol), morpholine hydrochloride (265 mg, 2.14 mmol), 1-hydroxybenzotriazol (338 mg, 2.50 mmol), WSC HCl (484 mg, 2.52 mmol), and triethylamine (0.37 ml, 2.65 mmol) in DMF (7 mL) was stirred for 1 h at room temperature. Water was added. The mixture was extracted with ethyl acetate-toluene, and the extracts were washed with water, dried over MgSO4, and concentrated. The residue was purified by silica gel column chromatography with 1:1 to 1:5 hexane/ethyl acetate to give the title compound (325 mg, 91%).
WORKUP
后处理
- extractionThe mixture was extracted with ethyl acetate-toluene
- washthe extracts were washed with water
- dry with materialdried over MgSO4
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography with 1:1 to 1:5 hexane/ethyl acetate