Reaktion #172423

ord-7af61dd6133245b29de4b35f1bc0b4fa

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated off
  2. 2
    Waschenthe residue was washed with ethanol
  3. 3
    SonstigeThe residue was purified by silica gel column chromatography
  4. 4
    Waschenwashed with ethanol

Vorschrift

In 8 ml of ethanol and 2.5 ml of tetrahydrofuran were dissolved 226 mg (0.61 mmol) of 5-[2-(4-dibutylamino-2-methoxyphenyl)vinyl]thiophene-2-carboaldehyde and 210 mg (0.62 mmol) of 2-(3-cyano-4-methyl-5-phenyl-5-trifluoromethyl-2(5H)-furanylidene)propanedinitrile. The mixture was stirred with heating at 70° C. for 4 hours. The solvent was evaporated off and the residue was washed with ethanol. The residue was purified by silica gel column chromatography and washed with ethanol to give 378 mg of a dark brown powdered crystal (yield: 92.9%; mp: 203-204° C.)

Quelle

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