HRID516989
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
2,4-dichloro phenol (138 mg, 0.85 mmol), 2-chloro-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone (compound 5, 0.3 g, 0.85 mmol) and anhydrous potassium carbonate (0.293 g, 2.125 mmol) were stirred for over night in dry acetonitrile (20 mL). The mixture was poured into a large volume of water and the solution extracted with diethyl ether. Un-reacted phenol was removed with cold 1N NaOH solution. The ether extract was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude material was purified by column chromatography to yield the title compound (350 mg, 87.5% yield) as an off-white solid.
WORKUP
后处理
- extractionthe solution extracted with diethyl ether
- customUn-reacted phenol was removed with cold 1N NaOH solution
- extractionThe ether extract
- dry with materialwas dried over anhydrous sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe crude material was purified by column chromatography