HRID2244218

反应详情

EQUATION

反应方程式

HRID 2244218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A stirred mixture containing 4.15 g (0.025 mole) of 2-bromothioanisole, 5.08 g. (0.0025 mole) of 4-carboxybenzeneboronic acid, 10.36 g (0.075 mol) of potassium carbonate and 0.45 g (0.00063 mol) of dichlorobis(triphenylphosphine)palladium(II) in 40 mL of water and 20 mL of 1,4-dioxane was heated under reflux for two hours under nitrogen. The reacton mixture was allowed to cool to room temperature and filtered. The dioxane was removed in vacuo, the residue was diluted with 100 mL of water and then acidified with 20% hydrochloric acid. The crude product (6.1 g) was recrystallized from ethanol to yield the title compound, m.p. 220-222° C.

WORKUP

后处理

  1. temperatureunder reflux for two hours under nitrogen
  2. filtrationfiltered
  3. customThe dioxane was removed in vacuo
  4. additionthe residue was diluted with 100 mL of water
  5. customThe crude product (6.1 g) was recrystallized from ethanol