반응 #45711

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7-Fluoro-2-[N-[[2-(4-methoxybenzyl)-2-H-[1,2,4]triazol-3-yl]methyl]methylamino]-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile

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solid

수율 97.4%

7-Fluoro-5-methyl-2-[methyl(1H-1,2,4-triazol-5-ylmethyl)amino]-6-phenyl-1,3-benzoxazole-4-carbonitrile

수율 97.4%

용매

trifluoroacetic acid

반응 조건

후처리

1. 1
   workup.WAITat an external temperature of about 60° C. for 6 hours
2. 2
   기타The solvent was evaporated away under reduced pressure
3. 3
   workup.ADDITIONethyl acetate and aqueous sodium hydrogencarbonate solution were added
4. 4
   기타the organic layer was separated
5. 5
   건조After drying over anhydrous sodium sulfate
6. 6
   기타the solvent was evaporated away under reduced pressure
7. 7
   기타the resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=20:1)

실험 절차

7-Fluoro-2-[N-[[2-(4-methoxybenzyl)-2-H-[1,2,4]triazol-3-yl]methyl]methylamino]-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-164) (0.33 g, 0.68 mmol) was dissolved in trifluoroacetic acid (5 ml), and stirred at room temperature for 16 hours, then at an external temperature of about 60° C. for 6 hours. The solvent was evaporated away under reduced pressure, then ethyl acetate and aqueous sodium hydrogencarbonate solution were added, and the organic layer was separated. After 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=20:1) to obtain a colorless solid (0.24 g, 97%).

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