HRID49330

反应详情

EQUATION

反应方程式

HRID 49330 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringAfter stirring for 20 minutes
  2. filtrationthe medium is then filtered
  3. concentrationThe filtrate is concentrated under reduced pressure
  4. customthe residue obtained
  5. customis then purified by chromatography on a column of silica