反应详情

To a solution of 33 (857 mg, 5.5 mmol), in DMF (14 mL) and DCM (25 mL) at room temperature, was added the hydrochloride of 1-amino-2-vinyl-cyclopropanecarboxylic acid ethyl ester, prepared as described in WO03/099274, (1.15 g, 6.0 mmol), HATU (2.29 g, 6.0 mmol) and DIPEA (3.82 mL, 22 mmol). The reaction was stirred under N2-atmosphere at ambient temperature for 1 h. LC/MS analysis showed complete conversion and the reaction mixture was concentrated in vacuo. The residue was redissolved in DCM (100 mL) and 0.1 M HCl (aq) and the phases were separated. The organic phase was washed with NaHCO3 (aq) and brine, dried (MgSO4) and filtered. Removal of the solvent in vacuo afforded the target compound (1.6 g, 99%). LC/MS>95%, m/z (ESI+)=294 (MH+)

1. customprepared
2. concentrationthe reaction mixture was concentrated in vacuo
3. dissolutionThe residue was redissolved in DCM (100 mL)
4. custom0.1 M HCl (aq) and the phases were separated
5. washThe organic phase was washed with NaHCO3 (aq) and brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customRemoval of the solvent in vacuo