반응 #45706

반응 방정식

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

ethyl isonipecotate

diisopropylethylamine

→

oil

수율 94.7%

Ethyl 1-(4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazol-2-yl)piperidine-4-carboxylate

수율 94.7%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도by heating
2. 2
   온도under reflux for 3 hours
3. 3
   세척washed with water
4. 4
   건조dried 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:methanol=100:1)

실험 절차

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-130) (0.20 g, 0.70 mmol) was dissolved in dichloromethane (10 ml), then ethyl isonipecotate (0.12 ml, 0.78 mmol) and diisopropylethylamine (0.15 ml, 0.88 mmol) were added, followed by heating under reflux for 3 hours. This was diluted with dichloromethane, washed with water, and dried 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=100:1) to obtain a yellow oil (0.27 g, 94%).

출처