Reaktion #45691

Reaktionsgleichung

N-methylethanolamine

diisopropylethylamine

N-methylethanolamine

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

→

oil

Ausbeute 93.0%

7-Fluoro-2-[(2-hydroxyethyl)(methyl)amino]-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile

Ausbeute 93.0%

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter heating
2. 2
   Temperaturunder reflux for 3 hours
3. 3
   TemperaturAfter heated
4. 4
   Temperaturunder reflux for 3 hours
5. 5
   WaschenAfter washing with water
6. 6
   Trocknendrying over anhydrous sodium sulfate
7. 7
   Sonstigethe solvent was evaporated away under reduced pressure
8. 8
   Sonstigethe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=40:1)

Vorschrift

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (0.20 g, 0.70 mmol) was dissolved in dichloromethane (10 ml), and diisopropylethylamine (0.13 ml, 0.76 mmol) and N-methylethanolamine (62.0 μl, 0.78 mmol) were added. After heating under reflux for 3 hours, N-methylethanolamine (62.0 μl, 0.78 mmol) was added. After heated under reflux for 3 hours, this was 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:methanol=40:1) to obtain a pale yellow oil (0.21 g, 93%).

Quelle