Reaktion #172500

ord-747163de371a4142b2f6a7dd3e0c992e

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe precipitate was separated by filtration
  2. 2
    Waschenwashed with methanol
  3. 3
    SonstigeThe crystal was purified by silica gel column chromatography
  4. 4
    Waschenwashed with methanol
  5. 5
    Sonstigeto give 228 mg of a dark blue crystal
  6. 6
    Sonstigeamp of 250-252° C. (yield: 85.2%)

Vorschrift

In 5 ml of ethanol were dissolved 150 mg (0.65 mmol) of 8-methoxy-2,3,6,7-tetrahydro-1H,5H-benzo[ij]quinolizine-9-carboaldehyde and 142 mg (0.71 mmol) of 2-(3-cyano-4,5,5-trimethyl-2(5H)-furanylidene)propanedinitrile. The mixture was stirred at room temperature for 3 hours and further at 50° C. for 3 hours. The precipitate was separated by filtration and washed with methanol. The crystal was purified by silica gel column chromatography and washed with methanol to give 228 mg of a dark blue crystal having amp of 250-252° C. (yield: 85.2%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846955B2uspto-grants-2014_09