Reaktion #10863

ord-baf1448600b24f08910c52ab2c44d07b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewhich was sealed
  2. 2
    Sonstigereacted at 20° C. for 40 hours
  3. 3
    Extraktionextracted (dichloromethane)
  4. 4
    Waschenwashed (water)
  5. 5
    Trocknendried (magnesium sulfate)
  6. 6
    Sonstigeevaporated
  7. 7
    Sonstigeto give a mixture which

Vorschrift

2-(2,6-Dichloro-4-trifluoromethylphenylhydrazono) succinonitrile (0.296 g, 1 mmol), sodium cyanide (0.196 g, 4 equivalents), water (1 ml) and acetic acid (5 ml) were added successively to a tube, which was sealed and reacted at 20° C. for 40 hours. The mixture was added to saturated sodium bicarbonate solution, extracted (dichloromethane), washed (water), dried (magnesium sulfate) and evaporated to give a mixture which contained 40% of the desired title compound, NMR 3.1 (m, 2H), 4.5 (m, 1H), 5.89 (m, 1H), 6.94 (d, 1H), 7.71 (s, 2H), together with 60% of unchanged starting hydrazone.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07094906B2uspto-grants-2006_08