반응 #45691

반응 방정식

N-methylethanolamine

diisopropylethylamine

N-methylethanolamine

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

→

oil

수율 93.0%

7-Fluoro-2-[(2-hydroxyethyl)(methyl)amino]-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
   온도After heated
4. 4
   온도under reflux for 3 hours
5. 5
   세척After washing with water
6. 6
   건조drying 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:methanol=40:1)

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 (0.13 ml, 0.76 mmol) and N-methylethanolamine (62.0 μl, 0.78 mmol) were added. After heating under reflux for 3 hours, N-methylethanolamine (62.0 μl, 0.78 mmol) was added. After heated under reflux 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:methanol=40:1) to obtain a pale yellow oil (0.21 g, 93%).

출처