반응 #45699

반응 방정식

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

diisopropylethylamine

azetidine-3-carbonyldimethylamide hydrochloride

→

oil

수율 86.9%

1-{4-Cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazol-2-yl}-N,N-dimethylazetidine-3-carboxamide

수율 86.9%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도After heated
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 to dichloromethane:methanol=100:1)

실험 절차

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (0.21 g, 0.73 mmol), (diisopropylethylamine (0.28 ml, 1.65 mmol) and azetidine-3-carbonyldimethylamide hydrochloride (I-145) (0.25 g) were dissolved in dichloromethane (10 ml). After heated under reflux for 3 hours, this was diluted with dichloromethane, washed with water, then 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 to dichloromethane:methanol=100:1) to obtain a colorless oil (0.24 g, 86%)

출처