HRID351817

反应详情

EQUATION

反应方程式

HRID 351817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 2 g (16.38 mmol) of 4-hydroxybenzaldehyde in 100 mL of DMF, 2.72 g (19.69 mmol) of K2CO3, 2.74 g (16.52 mmol) of KI and 3.94 mL (39.38 mmol) of 2-iodopropane was added under argon. The mixture was stirred at 80° C. overnight, concentrated and the residue obtained was partitioned between CHCl3 and H2O. The phases were separated, the aqueous phase was extracted with CHCl3 and the combined organic phases were dried over MgSO4 and concentrated. The crude product obtained was purified by chromatography on silica gel using EtOAc/hexane mixtures of increasing polarity as eluent, to give 2.08 g of the title compound of the example as an oil (77% yield).

WORKUP

后处理

  1. concentrationconcentrated
  2. customthe residue obtained
  3. customwas partitioned between CHCl3 and H2O
  4. customThe phases were separated
  5. extractionthe aqueous phase was extracted with CHCl3
  6. dry with materialthe combined organic phases were dried over MgSO4
  7. concentrationconcentrated
  8. customThe crude product obtained
  9. customwas purified by chromatography on silica gel
  10. temperatureof increasing polarity as eluent