반응 #3401

ord-e4c5a915e9a24293aae0af7d3e5b3bcb

시약

없음

반응 조건

온도
-18°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while maintaining the temperature below -10° C
  2. 2
    workup.WAITstored at 5° C. overnight
  3. 3
    workup.ADDITIONThe solution was then poured
  4. 4
    기타The precipitate was collected
  5. 5
    세척washed
  6. 6
    기타recrystallized from EtOH

실험 절차

Benzaldehyde (10.0 g, 94.2 mmol) and nitromethane (5.1 mL, 94.2 mmol) were dissolved in MeOH, the solution was cooled to -18° C., and NaOH (3.9 g, 98.9 mmol) in aqueous solution (80 mL) was added while maintaining the temperature below -10° C. The mixture was stirred at 0° C. for 2 hours, then stored at 5° C. overnight. The solution was then poured into stirring acid (200 mL conc. HCl/300 mL H2O). The precipitate was collected, washed, and recrystallized from EtOH to afford the title compound as light orange needles (5.15 g, 37%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733912uspto-grants-1998_03