반응 #1563945

ord-82f7c9d0ea5a40e68d3855443c41f360

반응 방정식

O=[N+]([O-])O
HNO3
CC(=O)c1cc(F)ccc1O
1-(5-fluoro-2-hydroxyphenyl)ethanone
CC(=O)c1cc(F)cc([N+](=O)[O-])c1O
1-(5-fluoro-2-hydroxy-3-nitrophenyl)ethanone

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction mixture was quenched with ice cold water
  2. 2
    여과The separated solid was filtered
  3. 3
    세척washed with cold water
  4. 4
    기타dried

실험 절차

Conc. HNO3 (22.49 g, 357 mmol) was added to a solution 1-(5-fluoro-2-hydroxyphenyl)ethanone (50 g, 325 mmol) in acetic acid (300 mL) at 0° C. and stirring was continued at 20° C. for 3 h. The reaction mixture was quenched with ice cold water. The separated solid was filtered and washed with cold water and dried to afford 1-(5-fluoro-2-hydroxy-3-nitrophenyl)ethanone (Int-49) as pale yellow solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 12.6 (1H, s), 8.3-8.2 (1H, dd), 8.2-8.1 (1H, dd), 2.7 (3H, s).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09402833B2uspto-grants-2016_08