반응 #80929

ord-68071ff8562a46d1ad8c90a9acf94b0f

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for about 17 hours
  2. 2
    온도The reaction mixture was cooled
  3. 3
    여과The resultant solid was collected by filtration
  4. 4
    세척was thoroughly washed with water
  5. 5
    기타The solid was dried at about 60° C. under vacuum

실험 절차

A stirred solution of 22.4 grams (0.106 mole) of 5-fluoro-2-methylcarbonylamino-3-methylnitrobenzene, 100 mL of concentrated hydrochloric acid, and 100 mL of ethanol was heated at reflux for about 17 hours. The reaction mixture was cooled and poured into 500 grams of ice. The mixture was made basic with aqueous 50% sodium hydroxide. The resultant solid was collected by filtration and was thoroughly washed with water. The solid was dried at about 60° C. under vacuum, yielding 17.0 grams of 4-fluoro-2-nitro-6-methylaniline, mp 111°-113° C. The NMR spectrum was consistent with the proposed structure. The reaction was repeated to obtain more product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05616718uspto-grants-1997_04