HRID2039156

反应详情

EQUATION

反应方程式

HRID 2039156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

The solution of 3-Methyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzoic acid methyl ester (3.71 g, 13.4 mmol), NBS (2.39 g, 13.4 mmol), and AIBN (235 mg) in CCl4 (20 ml) was heated at 80° C. for 14 hours. The mixture was cooled to 25° C., and was filtered and washed with CCl4. The solution was concentrated under reduced pressure, and was diluted with EtOAc. The solution was washed with water and brine and was dried with Na2SO4. Concentration gave 3-Bromomethyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzoic acid methyl ester (4.9 g).

WORKUP

后处理

  1. filtrationwas filtered
  2. washwashed with CCl4
  3. concentrationThe solution was concentrated under reduced pressure
  4. additionwas diluted with EtOAc
  5. washThe solution was washed with water and brine
  6. dry with materialwas dried with Na2SO4
  7. concentrationConcentration