반응 #45689

반응 방정식

N-methyl-tert-butylamine

diisopropylethylamine

N-methyl-tert-butylamine

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

→

solid

수율 93.0%

2-(N-tert-Butyl-N-methylamino)-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile

수율 93.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도After heating
2. 2
   온도under reflux for 3 hours
3. 3
   온도by heating
4. 4
   온도under reflux for 2 hours
5. 5
   세척washed with water
6. 6
   건조dried over anhydrous sodium sulfate
7. 7
   기타The solvent was evaporated away under reduced pressure
8. 8
   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 N-methyl-tert-butylamine (0.10 ml, 0.84 mmol) were added. After heating under reflux for 3 hours, N-methyl-tert-butylamine (50.0 μl, 0.42 mmol) was added, followed by heating under reflux for 2 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) to obtain a pale yellow solid (0.22 g, 0.65 mmol, 93%).

출처