Reaktion #1831458

Reaktionsgleichung

hexane acetone

3-[(4,4,4-Trifluoro-3-oxo-1-butenyl)amino]-2-propenenitrile

potassium hydroxide

→

title compound

Ausbeute 52.6%

4-Trifluoromethylnicotinamide

Ausbeute 52.6%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated
2. 2
   Temperaturunder reflux for 6 hours
3. 3
   EinengenThe reaction solution was concentrated under reduced pressure
4. 4
   SonstigeThe resulting residue was purified by silica gel column chromatography (a eluting solvent

Vorschrift

3-[(4,4,4-Trifluoro-3-oxo-1-butenyl)amino]-2-propenenitrile (a mixture of IIa and IIb; 1.90 g, 10 mmol) was dissolved in methanol (15 ml), and potassium hydroxide (990 mg, 15 mmol) was added. The mixture was heated under reflux for 6 hours. The reaction solution was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (a eluting solvent: hexane/acetone=1/1) to obtain 1.03 g (yield 52.6%) of the title compound.

Quelle