HRID1175763
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 solution of 1-Phenylthiocyclobutane-1-acetic acid (10 mmol) in benzene was treated with excess of PCl5 at room temperature for 15 h. The reaction mixture was concentrated under vacuum and the residue was again dissolved in benzene. AlCl3 was then added to the solution and it was stirred for 24 h at room temperature. The reaction mixture was diluted with excess of ethyl acetate and washed with water and brine. Organic layer was then separated, dried over anhydrous Na2SO4 and concentrated under vacuum. The residue was purified by column chromatography to afford the desired compound as oil.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under vacuum
- dissolutionthe residue was again dissolved in benzene
- additionAlCl3 was then added to the solution and it
- additionThe reaction mixture was diluted with excess of ethyl acetate
- washwashed with water and brine
- customOrganic layer was then separated
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated under vacuum
- customThe residue was purified by column chromatography