반응 #45687

반응 방정식

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

diisopropylethylamine

piperidine

→

solid

수율 90.0%

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

수율 90.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도This was heated
2. 2
   온도under reflux for 3 hours
3. 3
   세척After washing with water
4. 4
   건조drying over anhydrous sodium sulfate
5. 5
   기타the solvent was evaporated away under reduced pressure
6. 6
   기타the resulting residue was purified by silica gel column chromatography (dichloromethane)

실험 절차

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 (0.15 ml, 0.88 mmol) and piperidine (83.0 μl, 0.84 mmol) were added. This was heated under reflux for 3 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 obtain a colorless solid (0.21 g, 90%).

출처