HRID2071043

反应详情

EQUATION

反应方程式

HRID 2071043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a degassed mixture of 5.0 g (17.9 mmol) of 3,5-dibromophenylboronic acid in 50 mL of THF and 25 mL of 2 M Na2CO3 (aqueous) was added 1.13 g (0.975 mmol) of Pd(PPh3)4 and 2.3 mL of 2-bromopropene. The mixture was stirred at 40° C. for 5 h, and the mixture was extracted with EtOAc. The organic layer was washed with 25 mL of brine, dried over Na2SO4, filtered, and concentrated. Purification by flash silica gel chromatography (10% EtOAc/hexanes) provided 1,3-dibromo-5-(prop-1-en-2-yl)benzene with some impurity.

WORKUP

后处理

  1. extractionthe mixture was extracted with EtOAc
  2. washThe organic layer was washed with 25 mL of brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by flash silica gel chromatography (10% EtOAc/hexanes)