HRID249737

反应详情

EQUATION

反应方程式

HRID 249737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

3-Bromo-5-ethyl-6-methoxy-2-methylpyridine (11.51 g, 50 mmol), 4,4,5,5-tetramethyl-1,3,2-dioxaborolane (8.31 g, 64.95 mmol) and triethylamine (21.84 ml, 164.4 mmol) were dissolved under argon in 100 ml of dioxane and then 1,1′bis(diphenylphosphino)ferrocenepalladium(II) chloride (1.94 g, 2.65 mmol) was added. The mixture was stirred at 90° C. for 18 h, cooled and diluted with ethyl acetate, and filtered through silica gel. The solution was cooled to 0° C., mixed with water and extracted twice with ethyl acetate. The dried and concentrated organic phase was chromatographed on silica gel dried at 45° C. in a vacuum drying oven. A pale beige solid (9.94 g, 72%) was obtained.

WORKUP

后处理

  1. temperaturecooled
  2. filtrationfiltered through silica gel
  3. temperatureThe solution was cooled to 0° C.
  4. additionmixed with water
  5. extractionextracted twice with ethyl acetate
  6. customThe dried
  7. customconcentrated organic phase was chromatographed on silica gel
  8. customdried at 45° C. in a vacuum
  9. customdrying oven