HRID599690

反应详情

EQUATION

反应方程式

HRID 599690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 5-(1-ethyl-propenyl)-2-fluoro-benzaldehyde (8.70 g, 45.3 mmol) in DMF (40 mL) is treated with mercapto-acetic acid ethyl ester (8.16 g, 67.9 mmol) and K2CO3 (12.5 g, 90.6 mmol). The resulting suspension is stirred at 80° C. for 60 min and quenched with water (300 mL). The mixture is extracted with EtOAc (2×200 mL), and the organic layer is dried over Na2SO4, concentrated, and purified using silica gel column chromatography (6% EtOAc/Hex), to give the title compound as an oil (11.0 g, 89%).

WORKUP

后处理

  1. customquenched with water (300 mL)
  2. extractionThe mixture is extracted with EtOAc (2×200 mL)
  3. dry with materialthe organic layer is dried over Na2SO4
  4. concentrationconcentrated
  5. custompurified