Реакция #43994

ord-08ae92f127f94ec6a8ff8f48fe108716

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe white solid was filtered
  2. 2
    Промывкаwashed with water
  3. 3
    workup.DISSOLUTIONdissolved in dichloromethane (800 ml)
  4. 4
    ПромывкаThe solution was washed with water, brine
  5. 5
    Сушкаdried (MgSO4)
  6. 6
    Другоеthe solvent evaporated under vacuum

Методика

1,4-Diethoxy-2,3-naphthalenedicarboxylic anhydride (23.3 g, 81.5 mmol) and ethyl (4-aminophenyl)acetate (14.8 g, 82 mmol) were refluxed under nitrogen in acetic acid (160 ml) overnight. The mixture was cooled to room temperature and poured into water (1 L). The white solid was filtered, washed with water and dissolved in dichloromethane (800 ml). The solution was washed with water, brine and dried (MgSO4) and the solvent evaporated under vacuum to give ethyl[4-(4,9-diethoxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetate as an off-white solid, 33 g, 96%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07732622B2uspto-grants-2010_06