Reaktion #45685

Reaktionsgleichung

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile

diisopropylethylamine

pyrrolidine

→

oil

Ausbeute 98.0%

7-Fluoro-5-methyl-6-phenyl-2-(pyrrolidin-1-yl)-1,3-benzoxazole-4-carbonitrile

Ausbeute 98.0%

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThis was heated
2. 2
   Temperaturunder reflux for 4 hours
3. 3
   WaschenAfter washing with water
4. 4
   Trocknendrying over anhydrous sodium sulfate
5. 5
   Sonstigethe solvent was evaporated away under reduced pressure
6. 6
   Sonstigethe resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=100:1)

Vorschrift

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (0.13 g, 0.45 mmol) was dissolved in dichloromethane (10 ml), and diisopropylethylamine (92.0 μl, 0.54 mmol) and pyrrolidine (41.0 μl, 0.50 mmol) were added. This was heated under reflux for 4 hours, and diluted with dichloromethane. After washing with water and drying over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure, and the resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=100:1) to obtain a pale yellow oil (0.14 g, 98%).

Quelle