Trifluoroacetic acid → HCID 10211523, compound

Participants

Reaction Steps

The title compound was prepared according to the procedure described in Example 3 (Step b) from tert-butyl 3-{N-[(1R)-2-(4-(2-[(2-aminoethyl)-(methylsulfonyl)amino]phenyl}piperidyl)-1-[(4-chlorophenyl)methyl]-2-oxoethyl]carbamoyl}(3S)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate (Step f) (294.8 mg, 0.4 mmol) and 50% TFA in CH2Cl2 (20 mL). Purification by reverse phase preparative HPLC [Phenomenex; 5 μm 250×21.2 mm, 5% to 95% CH3CN (0.1% TFA) in H2O (0.1% TFA) over 30 min, then 100% CH3CN (0.1% TFA) for 2 min] provided the title compound (TFA salt) as a white solid (224 mg). MS (ESI, pos. ion) m/z: 638 (M+1); (ESI, neg. ion) m/z: 636 (M−1). Calc'd for C33H40ClN5O4S: 637.25. Anal. Calcd for C33H40ClN5O4S.2.5C2H3O2: C, 49.43; H, 4.64; N, 7.41. Found: C, 49.39; H, 4.78; N, 7.58.

Provenance & Evidence