HRID709020

反应详情

EQUATION

反应方程式

HRID 709020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 5-bromo-2,3-dimethoxypyridine (0.50 g, 2.29 mmol), tripotassium phosphate (1.95 g, 9.17 mmol), tetrakistriphenylphosphine (0.27 g, 0.23 mmol) and (E)-4,4,5,5-tetramethyl-2-styryl-1,3,2-dioxaborolane (0.53 g, 2.29 mmol) was diluted with dioxane (6 ml) and water (1 ml) and heated in a microwave for 1 hour at 100° C. The reaction mixture was partitioned between ethyl acetate and water and the organics were dried (MgSO4), filtered and concentrated in vacuo to give yellow oil. The oil was purified by column chromatography (SiO2; 0-10% ethyl acetate in petrol) gave 2,3-dimethoxy-5-[(E)-2-phenylethenyl]pyridine as a colourless oil (116 mg, 21%).

WORKUP

后处理

  1. customThe reaction mixture was partitioned between ethyl acetate and water
  2. dry with materialthe organics were dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customto give yellow oil
  6. customThe oil was purified by column chromatography (SiO2; 0-10% ethyl acetate in petrol)