HRID1677200

反应详情

EQUATION

反应方程式

HRID 1677200 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Procedure VV: To a stirring solution of 2-Ethanesulfonyl-5-iodo-pyridine (1.0 mmol) and (4-carboxy-3-fluorophenyl)boronic acid (1.3 mmol) in dioxane (0.1M), add dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium dichloromethane complex (0.03 mmol) and 2M aqueous sodium carbonate (3.0 mmol). Heat the reaction to reflux for 4 hours. After this time, remove the heat and concentrate in vacuo. Wash with dichloromethane while extracting with water. Acidify the aqueous layer with 1N hydrochloric acid and extract with 10% isopropanol/dichloromethane four times. Combine the organics, dry with sodium sulfate, decant and concentrate in vacuo. MS (m/e): 310.3 (M+1)

WORKUP

后处理

  1. temperatureHeat
  2. customthe reaction
  3. temperatureto reflux for 4 hours
  4. customAfter this time, remove the
  5. temperatureheat
  6. concentrationconcentrate in vacuo
  7. washWash with dichloromethane
  8. extractionwhile extracting with water
  9. extractionextract with 10% isopropanol/dichloromethane four times
  10. dry with materialCombine the organics, dry with sodium sulfate
  11. customdecant
  12. concentrationconcentrate in vacuo