反应详情

To a mixture of (6RS,8SR)-6-{[tert-butyl(dimethyl)silyl]oxy}-8-(3,4-difluorophenyl)-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 (209 mg) in DMF (1.9 mL) was added sodium hydride (60%, 16.6 mg) at 0° C., and the mixture was stirred for 10 min. Paraformaldehyde (18.1 mg) was added to the reaction mixture, and the mixture was stirred at room temperature for 1 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. To a mixture of the residue in THF (1.9 mL) was added TBAF (1M THF solution, 0.756 mL), and the mixture was stirred at room temperature for 15 min. Saturated aqueous sodium chloride solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was washed with ethyl acetate to give the title compound (154 mg).

1. stirringthe mixture was stirred at room temperature for 1 hr
2. extractionthe mixture was extracted with ethyl acetate
3. dry with materialThe extract was dried over anhydrous magnesium sulfate
4. customthe solvent was evaporated under reduced pressure
5. additionTo a mixture of the residue in THF (1.9 mL)
6. additionwas added TBAF (1M THF solution, 0.756 mL)
7. stirringthe mixture was stirred at room temperature for 15 min
8. additionSaturated aqueous sodium chloride solution was added to the reaction mixture
9. extractionthe mixture was extracted with ethyl acetate
10. dry with materialThe extract was dried over anhydrous magnesium sulfate
11. customthe solvent was evaporated under reduced pressure
12. washThe residue was washed with ethyl acetate