반응 #45679

반응 방정식

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

diisopropylethylamine

dimethylamine

→

solid

수율 87.1%

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

수율 87.1%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   세척After washing with water
2. 2
   건조drying over anhydrous sodium sulfate
3. 3
   기타the solvent was evaporated away under reduced pressure
4. 4
   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 (7 ml), then diisopropylethylamine (0.15 ml, 0.88 mmol), dimethylamine (2.0 M tetrahydrofuran solution, 0.50 ml, 1.00 mmol) were added. After stirring in a sealed tube at an external temperature of about 60° C. 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) to obtain a colorless solid (0.18 g, 87%).

출처