HRID49330
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
12.7 g (31.5 mmol) of dimethyl 4-[5-(2-ethyl-[1,3]dioxolan-2-yl)-2-thienylmethoxy]phthalate are dissolved in 500 mL of anhydrous ethyl ether. 2.87 g (75.7 mmol) of lithium aluminium hydride are added and the reaction medium is stirred at 0° C. for 1 hour. 2.9 mL of water are then added slowly, followed by 2.9 mL of aqueous 15% sodium hydroxide, and then 8.7 mL of water are also added slowly. After stirring for 20 minutes, the medium is then filtered. The filtrate is concentrated under reduced pressure and the residue obtained is then purified by chromatography on a column of silica. A white solid (m.p.: 78-80° C.) is obtained (m=8 g; Y=72%).
WORKUP
后处理
- stirringAfter stirring for 20 minutes
- filtrationthe medium is then filtered
- concentrationThe filtrate is concentrated under reduced pressure
- customthe residue obtained
- customis then purified by chromatography on a column of silica