HRID1931432

反应详情

EQUATION

反应方程式

HRID 1931432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

5 g (24.6 mmol) of 2-bromo-5-nitro-pyridine, 3.79 g (27.1 mmol) of 2-fluoro-phenylboronic acid, 276.5 mg (1.23 mmol) of palladium acetate, 646 mg (2.46 mmol) of triphenylphosphine and 24.6 ml of a 1 M aqueous sodium carbonate solution in 150 ml of toluene and 37 ml of ethanol were heated under reflux for 5 h. After cooling, the mixture concentrated under reduced pressure to half of its volume, poured onto water and extracted with ethyl acetate. The combined organic phases were dried and evaporated. The product was purified by chromatography (silica gel, n-heptane/ethyl acetate 5:1). Yield: 4.2 g.

WORKUP

后处理

  1. temperatureunder reflux for 5 h
  2. temperatureAfter cooling
  3. concentrationthe mixture concentrated under reduced pressure to half of its volume
  4. additionpoured onto water
  5. extractionextracted with ethyl acetate
  6. customThe combined organic phases were dried
  7. customevaporated
  8. customThe product was purified by chromatography (silica gel, n-heptane/ethyl acetate 5:1)