反应 #59101

ord-26fff85136a04713bcbeefda0f73eb8a

反应条件

温度
-10°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他resulting solution
  2. 2
    温度to warm to room temperature
  3. 3
    其他Solution was quenched with 10% sodium sulfite
  4. 4
    萃取extracted with dichloromethane
  5. 5
    洗涤Organics were washed with brine
  6. 6
    干燥dried with sodium sulfate
  7. 7
    浓缩concentrated
  8. 8
    其他Crude product was purified with flash chromatography (85% Hex: 15% EtoAc)

实验过程

1-fluoro-4-nitro-2-(prop-1-en-2-yl) benzene (1 eq) was dissolved in dichloromethane and cooled to −10° C. using and ice/salt/water bath under nitrogen. MCPBA (1.5 eq) in dichloromethane was then added dropwise and resulting solution allowed to warm to room temperature and allowed to stir 48 h. Solution was quenched with 10% sodium sulfite, neutralized with saturated solution of sodium bicarbonate, extracted with dichloromethane. Organics were washed with brine, dried with sodium sulfate and concentrated. Crude product was purified with flash chromatography (85% Hex: 15% EtoAc) to afford 2-(2-fluoro-5-nitrophenyl)-2-methyloxirane.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07423150B2uspto-grants-2008_09