반응 #82642

ord-e3ea6d41cd944af5b399fa1e23324e63

용매

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITat room temperature for 3 h
  2. 2
    여과The precipitate was collected by filtration

실험 절차

To 2-acetamido-5-fluorobenzotrifluoride (1.369 g, 6.19 mmol) in concentrated H2SO4 (6 mL) at 0° C. was added dropwise 70% HNO3 (0.8 mL, Baker). The mixture was stirred at 0° C. for 0.5 h, then at room temperature for 3 h and it was poured into ice water (25 g). The precipitate was collected by filtration, affording 2.1 g of crude 2-acetamido-5-fluoro-3-nitrobenzotrifluoride. It was crystallized from EtOH/H2O to afford 1.50 g of pure compound as yellow needles.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05622952uspto-grants-1997_04