HRID219776

反应详情

EQUATION

反应方程式

HRID 219776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a solution of methyl 4-bromo-3-nitrobenzoate (Chess, 3 g, 11.53 mmol) in toluene (100 mL) and water (100 mL) was added o-tolylboronic acid (1.88 g, 13.84 mmol) followed by potassium carbonate (7.972 g, 57.68 mmol), tetrakis(triphenylphosphine)palladium(0) (0.668 g, 0.577 mmol). The reaction mixture was refluxed at 120° C. for 14 h. After the completion of reaction, it was cooled to RT and organic layer was separated and evaporated under reduced pressure. The crude compound was passed through silica pad (60-120 mesh) using hexane as eluent to give the title compound as a white solid (2.5 g, 79%). 1H NMR: (DMSO-d6, 400 MHz) δ 8.52 (s, 1H), 8.29-8.26 (m, 1H), 7.63-7.61 (m, 1H), 7.34-7.33 (m, 2H), 7.23 (m, 1H), 7.13 (m, 1H), 3.94 (s, 3H), 2.04 (s, 3H).

WORKUP

后处理

  1. customAfter the completion of reaction, it
  2. temperaturewas cooled to RT
  3. customorganic layer was separated
  4. customevaporated under reduced pressure