HRID49323
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
350 mg (0.76 mmol) of dimethyl 4-[5-((E)-5-ethyl-5-hydroxy-1-methylhept-1-enyl)-2-thienylmethoxy]phthalate are dissolved in 20 mL of anhydrous ethyl ether. 70 mg (1.8 mmol) of lithium aluminium hydride are added and the reaction medium is stirred at room temperature for 30 minutes. 400 mL of water are then added slowly and the medium is filtered. The filtrate is concentrated under reduced pressure and the residue obtained is then purified by chromatography on a column of silica (eluent: 70 ethyl acetate/30 heptane). A white solid (m.p.: 100-102° C.) is obtained (m=175 mg; Y=58%).
WORKUP
后处理
- filtrationthe medium is filtered
- concentrationThe filtrate is concentrated under reduced pressure
- customthe residue obtained
- customis then purified by chromatography on a column of silica (eluent: 70 ethyl acetate/30 heptane)