반응 #9457

ord-e52aec0cac81483fa1aff8a997e54a25

반응 조건

온도
129°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONdropped to 124° C
  2. 2
    온도cooled to 5° C. on an ice bath
  3. 3
    여과The resulting solid was collected by filtration
  4. 4
    세척washed with ice cold ethanol (until washings
  5. 5
    기타dried at 70° C. in a vacuum oven overnight

실험 절차

A stirred suspension of 7-phenylquinolin-4-ol (84.9 g, 384 mmol) in propionic acid (850 mL) was heated to 129° C. Nitric acid (70%, 45.0 g) was added dropwise over 25 min, during which the temperature dropped to 124° C. The reaction was stirred an additional 3 h at that temperature and then cooled to 5° C. on an ice bath. The resulting solid was collected by filtration, washed with ice cold ethanol (until washings were nearly colorless) and dried at 70° C. in a vacuum oven overnight to obtain 83.2 g of 3-nitro-7-phenylquinolin-4-ol as a beige powder.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091214B2uspto-grants-2006_08