HRID1640878

反应详情

EQUATION

反应方程式

HRID 1640878 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Combine 2-fluoro-5-iodo-pyridine (1.12 g, 5 mmol), cyclopropylboronic acid (645 mg, 7.5 mmol), palladium acetate (56 mg, 0.25 mmol) and potassium phosphate (3.2 g, 15 mmol) in toluene/water (20:1, 21 mL). Heat the mixture at 100° C. for 4 h. Dilute the mixture with chloroform-IPA (3:1, 100 mL). Wash the organic phase with saturated aqueous sodium chloride and water. Dry the mixture over sodium sulfate. Concentrate the solution in vacuo to a brown oil. Purify by column chromatography (20% ethyl acetate in hexane) to afford the title compound as a pale yellow oil (430 mg, 63%).

WORKUP

后处理

  1. washWash the organic phase with saturated aqueous sodium chloride and water
  2. dry with materialDry the mixture over sodium sulfate
  3. concentrationConcentrate the solution in vacuo to a brown oil
  4. customPurify by column chromatography (20% ethyl acetate in hexane)