HRID227235

反应详情

EQUATION

反应方程式

HRID 227235 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

4-Bromo-2-nitro-phenol (648 mg, 3.0 mmol) and 3-pyridyl boronic acid (387 mg, 3.15 mmol) were diluted with 5 mL of dioxane and placed under N2. Potassium carbonate was diluted in 1 mL of H2O and added to the reaction mixture. Tetrakis(triphenylphosphine) palladium (173 mg, 0.15 mmol) was added, then the reaction was heated to 70° C. and stirred overnight. The reaction was allowed to cool to room temperature, then diluted with 30 mL of EtOAc and 30 mL of 10% Na2CO3. The organic layer was washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The material was purified with a Biotage 40M cartridge eluting with hexanes/EtOAc, 1/1 to yield an off white solid.

WORKUP

后处理

  1. additionadded to the reaction mixture
  2. temperatureto cool to room temperature
  3. washThe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe material was purified with a Biotage 40M cartridge
  8. washeluting with hexanes/EtOAc, 1/1
  9. customto yield an off white solid