反应详情

Under an argon atmosphere, ethyl 3-[3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)phenyl]-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridine-8-carboxylate (1.00 g) was added to a suspension of sodium hydride (60%, 115 mg) in DMF (10 mL) under ice-cooling. The reaction mixture was stirred for 20 min under ice-cooling, N-chlorosuccinimide (383 mg) was added under ice-cooling, and the mixture was stirred for 20 min under ice-cooling. The reaction mixture was diluted with ethyl acetate, the mixture was poured into saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (methanol/ethyl acetate) to give the title compound (750 mg).

1. temperaturecooling
2. temperaturecooling
3. temperaturecooling
4. stirringthe mixture was stirred for 20 min under ice-
5. temperaturecooling
6. extractionthe mixture was extracted with ethyl acetate
7. washThe extract was washed with saturated brine
8. dry with materialdried over anhydrous sodium sulfate
9. customthe solvent was evaporated under reduced pressure
10. customThe residue was purified by silica gel column chromatography (methanol/ethyl acetate)