反应详情

温度

50 °C

1,1-dimethylethyl (1S,4S,6S)-4-(aminomethyl)-3-azabicyclo[4.1.0]heptane-3-carboxylate D29 (400 mg) and 2-bromo-5-(trifluoromethyl)pyrazine (401 mg, 1.767 mmol) were dissolved in DMF (2 ml) then sodium carbonate (375 mg, 3.53 mmol) was added and the mixture was heated to 50° C. for 2 hours. DMF was concentrated under vacuum and the residue was taken up with DCM (3 ml) and washed with NaHCO3 saturated solution (4 ml). The organic phase was filtered through a phase separator tube, concentrated under vacuum and purified by silica gel chromatography (Biotage SP—column size 25 g SNAP using Cy:EtOAc=8:2 to 2:8 as eluent). It was recovered the title compound D30 (300 mg).

1. concentrationDMF was concentrated under vacuum
2. washwashed with NaHCO3 saturated solution (4 ml)
3. filtrationThe organic phase was filtered through a phase separator tube
4. concentrationconcentrated under vacuum
5. custompurified by silica gel chromatography (Biotage SP—column size 25 g SNAP using Cy:EtOAc=8:2 to 2:8 as eluent)
6. customIt was recovered the title compound D30 (300 mg)