HRID1049433

反应详情

EQUATION

反应方程式

HRID 1049433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of (2′-fluoro-5′-methoxy-2-neopentyl-[1,1′-biphenyl]-4-yl)(4-methoxybenzyl)sulfane (1.68 g) in trifluoroacetic acid (6.6 mL) was added anisole (2.15 mL) at room temperature, and the mixture was stirred at 90° C. for 8 hr. The reaction mixture was cooled to 0° C., neutralized with 8N aqueous sodium hydroxide solution, and 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 (NH, ethyl acetate/hexane) to give the title compound (918 mg) as a pale-yellow oil.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. extractionextracted 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 (NH, ethyl acetate/hexane)