HRID572144

反应详情

EQUATION

反应方程式

HRID 572144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

To a solution of bromo-imidazo[1,2-a]pyridine derivatives (1.0 equiv.) in DMF, Zinc cyanide (1.1 equiv.) and Pd(PPh3)4 (5%) were added under inert atmosphere. The resulting mixture was heated through microwave irradiation for 10 min at 130° C. (Power max tolerated was 70 W). The yellow cloudy reaction mixture was hydrolyzed with HCl 1N solution then extracted with Et2O. Aqueous layer was cooled by an ice bath, and NaOH solid was added until a pH was greater than 10. The resulting aqueous basic layer was extracted with EtOAC. Organic layer was washed with brine, dried over MgSO4 and concentrated under reduced pressure.

WORKUP

后处理

  1. customThe yellow cloudy reaction mixture
  2. extractionthen extracted with Et2O
  3. temperatureAqueous layer was cooled by an ice bath
  4. additionNaOH solid was added until a pH was greater than 10
  5. extractionThe resulting aqueous basic layer was extracted with EtOAC
  6. washOrganic layer was washed with brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated under reduced pressure