HRID383077

反应详情

EQUATION

反应方程式

HRID 383077 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2-Bromo-4-nitrobenzoic acid (0.43 g, 2.03 mmol) and 3,5-dimethylphenyl boronic acid (0.334 g, 2.23 mmol) were dissolved in anhydrous DMF (25 mL) under nitrogen. To this mixture was added Cs2CO3 (1.66 g, 5.08 mmol) followed by Pd(Ph3P)4 (0.12 g, 5%). The mixture was heated at 100° C. overnight. The solution was poured onto 1N HCl and extracted with Et2O. It was dried over MgSO4 and the solvent was removed in vacuo. The crude product was chromatographed on silica gel using a 9:1 mixture of hexanes and ethyl acetate to provide the desired product (0.34 g):

WORKUP

后处理

  1. extractionextracted with Et2O
  2. dry with materialIt was dried over MgSO4
  3. customthe solvent was removed in vacuo
  4. customThe crude product was chromatographed on silica gel using
  5. additiona 9:1 mixture of hexanes and ethyl acetate