HRID1066434
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
To a stirred mixture of 2.7 g (10 mmol) of 2-(4-methoxy-benzenesulfonyl)propionic acid ethyl ester, 3.03 gm (10 mmol) 4-(2-piperidin-1-yl-ethoxy)benzyl chloride, 10 gm of K2CO3 and 500 mg of 18-crown-6 in 250 ml of acetone was refluxed for 16 hours. At the end, the reaction mixture was filtered and the acetone layer was concentrated to a residue. The residue was extracted with chloroform, washed well with water, dried over anhydrous MgSO4, filtered and concentrated to a residue. The residue obtained was purified by silica-gel column chromatography by eluting with 50% ethyl acetate-hexanes to afford 4.8 gm (92%) of the desired product as an oil. MS: 490(M+H)+.
WORKUP
后处理
- temperaturewas refluxed for 16 hours
- filtrationAt the end, the reaction mixture was filtered
- concentrationthe acetone layer was concentrated to a residue
- extractionThe residue was extracted with chloroform
- washwashed well with water
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered
- concentrationconcentrated to a residue
- customThe residue obtained
- customwas purified by silica-gel column chromatography
- washby eluting with 50% ethyl acetate-hexanes