HRID1470630

反应详情

EQUATION

反应方程式

HRID 1470630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of toluene (30 mL) and water (5 mL) was degassed with nitrogen for 30 min. A mixture of sodium carbonate (2.26 g, 6.9 mmol) was added followed by 2-methoxy-4-bromobenzaldehyde (0.5 g, 2.3 mmol), phenylboronic acid (0.337 g, 2.7 mmol) and tetrakis triphenyl phosphene palladium(0) (0.261 g, 0.022 mmol) to the above degassed water/toluene mixture. The reaction mixture was then refluxed overnight. After the reaction is completed, it was cooled to room temperature and extracted with ethyl acetate. The combined organic layers were dried over sodium sulphate and concentrated. The obtained residue was purified by column chromatography using 3% ethyl acetate in hexane to obtain the title compound.

WORKUP

后处理

  1. customwas degassed with nitrogen for 30 min
  2. additionwas added
  3. customabove degassed water/toluene mixture
  4. temperatureThe reaction mixture was then refluxed overnight
  5. extractionextracted with ethyl acetate
  6. dry with materialThe combined organic layers were dried over sodium sulphate
  7. concentrationconcentrated
  8. customThe obtained residue was purified by column chromatography