Réaction #527476

ord-b156d6597c04481d8cf0e5949113d61a

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreThe precipitate formed
  2. 2
    Filtrationwas filtered
  3. 3
    Lavagewashed with 3×10 ml of distilled water
  4. 4
    Autredried

Mode opératoire

1.3 g (4.4 mmol) of 1-(4-aminophenyl)-3-acetyl-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine were stirred at 20°-25° C. with 5 ml of acetic anhydride for one hour, then the yellow solution was poured into 100 g of ice-water and stirred until the decomposition of the excess anhydride became complete. The precipitate formed was filtered, washed with 3×10 ml of distilled water and dried to give 1.6 g of raw product. After recrystallization from 20 ml of benzene 1.50 g (89.85%) of the aimed product were obtained, m.p.: 158°-160° C. (decomp.).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05519019uspto-grants-1996_05