反应详情

2.10 g (8.36 mmol) tert. butyl 7,7-dimethyl-1,4,6,7-tetrahydro-pyrazolo[4,3-c]pyridine-5-carboxylate were placed in 25 mL DMF. While cooling with ice, 350 mg (8.75 mmol) sodium hydride (55%) were added. The reaction mixture was stirred for 30 min, then 0.540 mL (8.67 mmol) iodomethane were added and the mixture was stirred for 1 h at 0° C. The reaction mixture was concentrated to dryness by rotary evaporation and the residue was mixed with water and extracted with EtOAc. The organic phase was dried, filtered and concentrated to dryness by rotary evaporation. The residue was purified by HPLC. The product-containing fractions were combined and organic solvent was eliminated by rotary evaporation. The aqueous residue was extracted with DCM. The organic phase was dried, filtered and concentrated to dryness by rotary evaporation.

1. additionwere added
2. stirringthe mixture was stirred for 1 h at 0° C
3. concentrationThe reaction mixture was concentrated to dryness by rotary evaporation
4. additionthe residue was mixed with water
5. extractionextracted with EtOAc
6. customThe organic phase was dried
7. filtrationfiltered
8. concentrationconcentrated to dryness by rotary evaporation
9. customThe residue was purified by HPLC
10. customorganic solvent was eliminated by rotary evaporation
11. extractionThe aqueous residue was extracted with DCM
12. customThe organic phase was dried
13. filtrationfiltered
14. concentrationconcentrated to dryness by rotary evaporation