1,2-Dichloroethane → HCID 11294495, compound

Participants

Reaction Steps

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.

Provenance & Evidence