HRID1049601

反应详情

EQUATION

反应方程式

HRID 1049601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Under a nitrogen atmosphere, to a mixture of sodium hydride (60%, 133 mg) and THF (20 mL) was added diethyl cyanomethylphosphonate (0.54 mL) at 0° C., and the mixture was stirred at 0° C. for 10 min. To the reaction mixture was added 2′-fluoro-5′-methoxy-4-((4-methoxybenzyl)oxy)biphenyl-2-carbaldehyde (1.03 g) obtained in Example 93, step 2, and the mixture was stirred at 50° C. for 30 min. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give a crude product of the title compound as a colorless oil. This compound was used for the next step without further purification.

WORKUP

后处理

  1. stirringthe mixture was stirred at 50° C. for 30 min
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)