HRID409720

反应详情

EQUATION

反应方程式

HRID 409720 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under inert gas atmosphere 36 mg (0.049 mmol) PdCl2(dppf)xCH2Cl2, 28 mL (56 mmol) 2N sodium carbonate solution and 3.35 g (27.2 mmol) pyridine-4-boronic acid are added to 7.50 g (24.7 mmol) N-ethyl-2-(4-iodo-phenyl)-propionamide (V1.1) in 45 mL 1,4-dioxane and 15 mL methanol. The mixture is stirred for 2 d at reflux. After that time, water is added and the mixture is extracted with EtOAc (2×). The combined organic layers are washed with water and 150 mL 1N HCl are added. The aq. layer is separated, filtered and alkalized with 1N NaOH. The precipitate is filtered off and dried.

WORKUP

后处理

  1. temperatureat reflux
  2. extractionthe mixture is extracted with EtOAc (2×)
  3. washThe combined organic layers are washed with water and 150 mL 1N HCl
  4. additionare added
  5. customThe aq. layer is separated
  6. filtrationfiltered
  7. filtrationThe precipitate is filtered off
  8. customdried