Réaction #172508

ord-aa904c33c98c433fa27ac7ea2aa63a45

Solvants

Conditions de réaction

Température
80°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrethe precipitate was separated by filtration
  2. 2
    Lavagewashed with water
  3. 3
    Autredried
  4. 4
    AutreThe crystal was purified by silica gel column chromatography
  5. 5
    Lavagewashed with methanol

Mode opératoire

In 10 ml of anhydrous acetic acid were dissolved 0.8 g (3.04 mmol) of 4-(dibutylamino)-2-methoxybenzaldehyde and 0.73 g (3.01 mmol) of 1,3-bis(dicyanomethylidene)indan. The mixture was stirred with heating at 80° C. for 2 hours. The reaction mixture was poured into 200 ml of water and the precipitate was separated by filtration, washed with water, and dried. The crystal was purified by silica gel column chromatography and washed with methanol to give 1.27 g of a black crystal having a mp of 195-198° C. (yield: 86.4%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08846955B2uspto-grants-2014_09