Реакция #2047

ord-f7732a0ba48b458e9add51628a8da0ea

Уравнение реакции

Nc1ccc2c3c(cccc13)CC2
5-aminoacenaphthene
CC(=O)OC(C)=O
acetic anhydride
Nc1ccc2c3c(cccc13)CC2
5-aminoacenaphthene
CC(=O)Nc1ccc2c3c(cccc13)CC2
5-(N-acetylamino)acenaphthene
Выход 96.4%

Растворители

Условия реакции

Температура
60°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.DISSOLUTIONto dissolve
  2. 2
    workup.ADDITIONthe dropwise addition
  3. 3
    workup.STIRRINGthe mixture was stirred at the same temperature for 2 hours
  4. 4
    Другоеto precipitate a crystal, which
  5. 5
    Фильтрацияwas then filtrated
  6. 6
    Промывкаwashed with water
  7. 7
    Другоеdried

Методика

50 ml of glacial acetic acid was added to 6.77 g (0.04 mol) of 5-aminoacenaphthene and the mixture was stirred at 60° C. to dissolve, and 8.16 g (0.08 mol) acetic anhydride was dropwise added thereto for 15 minutes. After finishing the dropwise addition, the mixture was stirred at the same temperature for 2 hours. The reaction was determined to be finished when disappearance of 5-aminoacenaphthene was identified. The reaction product was poured into 500 ml of ice water to precipitate a crystal, which was then filtrated, washed with water and dried. As this result, 8.15 g (yield: 96.4%, melting point: 180.0°-186.0° C.) of 5-(N-acetylamino)acenaphthene was obtained.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05728500uspto-grants-1998_03