Реакция #1797493

ord-7573a06fde9e4be5af8da2e0a35cb8d9

Реагенты

Нет

Растворители

Условия реакции

Температура
50°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONAfter completion of the dropwise addition
  2. 2
    ДругоеAfter completion of the reaction
  3. 3
    Другоеthe reaction liquid
  4. 4
    workup.STIRRINGwhile stirring
  5. 5
    ДругоеCrystals precipitated
  6. 6
    Фильтрацияwere filtered off
  7. 7
    Промывкаwashed with 1,000 ml of water
  8. 8
    ДругоеThe crystals obtained
  9. 9
    Другоеwere dried

Методика

33.3 g (0.25 mol) of 5-aminoindane (a product of Tokyo Chemical Industry Co. Ltd.) was dissolved in 250 ml of glacial acetic acid, the resulting solution was heated to 50° C., and 51.0 g (0.5 mol) of acetic anhydride was added dropwise thereto. After completion of the dropwise addition, the resulting solution was stirred for 4 hours. After completion of the reaction, the reaction liquid was poured in 1,500 ml of ice water while stirring. Crystals precipitated were filtered off, and washed with 1,000 ml of water. The crystals obtained were dried to obtain 37.06 g of 5-(N-acetylamino)indane (yield: 84.6%, melting point: 100.5 to 103.5° C.)

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07790342B2uspto-grants-2010_09