HRID1186947

反应详情

EQUATION

反应方程式

HRID 1186947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 5-bromo-2-benzofuran-1(3H)-one (15.0 g, 70.4 mmol), allyl-tributyl-stannane (25.6 g, 77.5 mmol), LiCl (11.8 g, 282 mmol) and Pd(PPh3)4 (1.2 g, 1.0 mmol) in 100 mL toluene was heated under N2 at 90˜100° C. overnight. After cooling to r.t., the mixture was diluted with 250 mL EtOAc and filtered. The filtrate was washed with water and brine, dried over anhydrous Na2SO4 and concentrated to dryness. The residue was purified via column (DCM/Petrol Ether=1:5) to give 5-prop-2-en-1-yl-2-benzofuran-1(3H)-one.

WORKUP

后处理

  1. temperaturewas heated under N2 at 90˜100° C. overnight
  2. filtrationfiltered
  3. washThe filtrate was washed with water and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated to dryness
  6. customThe residue was purified via column (DCM/Petrol Ether=1:5)