HRID1896691

反应详情

EQUATION

反应方程式

HRID 1896691 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A mixture of 1000 mg (3.87 mmol) of 3-(6-bromopyridin-3-yl)propionic acid ethyl ester, 596.3 mg (4.26 mmol) of 2-fluorophenylboronic acid, 43.5 mg (0.19 mmol) of palladium acetate, 101.6 mg (0.38 mmol) of triphenylphosphane, 3.88 ml of a 1M sodium carbonate solution, 23 ml of toluene and 6 ml of ethanol was heated under reflux for 5 h and, after cooling, poured into water. The resulting mixture was extracted with ethyl acetate. The organic phase was separated and concentrated, and the residue was purified by chromatography (silica gel, n-heptane/ethyl acetate 5:1). Yield: 782 mg (74%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 h
  3. temperatureafter cooling
  4. extractionThe resulting mixture was extracted with ethyl acetate
  5. customThe organic phase was separated
  6. concentrationconcentrated
  7. customthe residue was purified by chromatography (silica gel, n-heptane/ethyl acetate 5:1)