反应详情

To a solution of the title compound of Example 1 Step D (0.1 mmol, 41 mg), the hydrochloride salt of β-alanine tert-butyl ester (0.15 mmol, 27 mg), HOBt (0.25 mmol, 38 mg) and EDC (0.4 mmol, 77 mg) in 1 mL of DMF was added DIEA (0.5 mmol, 90 μL). The reaction mixture was allowed to stand at ambient temperature overnight, then partitioned into EtOAc/H2O. The aqueous phase was washed with EtOAc, and the combined organic phase was dried with MgSO4 and the solvent was removed under reduced pressure. The residue was treated with 3 mL of 2:30:68H2O/TFA/DCM for 1 hr and the solution was concentrated under reduced pressure. Purification by reverse-phase chromatography (Condition A), followed by lyophilization, afforded the product as a white solid. MS (ESI): m/z 477 (M+H). HPLC A: 1.70 min.

1. custompartitioned into EtOAc/H2O
2. washThe aqueous phase was washed with EtOAc
3. dry with materialthe combined organic phase was dried with MgSO4
4. customthe solvent was removed under reduced pressure
5. additionThe residue was treated with 3 mL of 2:30:68H2O/TFA/DCM for 1 hr
6. concentrationthe solution was concentrated under reduced pressure
7. customPurification by reverse-phase chromatography (Condition A),