HRID1466156

反应详情

EQUATION

反应方程式

HRID 1466156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To an ice-bath cooled flask containing a solution of (2E)-3-(1-oxo-1,3-dihydro-2-benzofuran-5-yl)prop-2-enal (5 g, 26.6 mmol) in THF (20 mL) and methanol (20 mL) was added NaBH4 (1 g, 26.3 mmol), and the mixture was stirred for 1 hour at 0° C. The reaction mixture was then diluted with HCl (2 N, 20 mL) and extracted with EtOAc (300 mL). The organic layer was washed with water (30 mL) and brine (30 mL), dried over Na2SO4, and concentrated in vacuo. The residue was purified with silica gel chromatography (pet ether/EtOAc=2:1) to give the title product.

WORKUP

后处理

  1. temperatureTo an ice-bath cooled flask
  2. extractionextracted with EtOAc (300 mL)
  3. washThe organic layer was washed with water (30 mL) and brine (30 mL)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified with silica gel chromatography (pet ether/EtOAc=2:1)