Trifluoroacetic acid → HCID 6914611, compound

Participants

Reaction Steps

A solution of Example 27B (0.125 g, 0.25 mmol) in dichloromethane (3 mL) at room temperature was treated with TFA (400 μL), stirred for 1 hour, and concentrated. The concentrate was azeotropically distilled with diethyl ether two times and the residue was purified by reverse phase HPLC on a C18 column with 0-100% CH3CN/H2O/0.1% TFA to provide the desired product as the di-trifluoroacetate salt (0.110 g, 70%). MS (ESI) m/e 395 (M+H)+; 1H NMR (DMSO-d6, 300 MHz) δ 11.02 (br s, 1H), 9.52 (s, 1H), 8.76 (d, J=3 Hz, 1H), 8.62 (d, J=8 Hz, 1H), 8.44-8.46 (m, 2H), 8.38 (d, J=9 Hz, 1H), 8.11-8.20 (m, 3H), 8.04-8.08 (m, 1H), 7.83-7.86 (m, 1H), 7.62 (d, J=9 Hz, 1H), 7.37-7.40 (m, 1H), 7.31 (d, J=3 Hz, 1H), 7.08-7.12 (m, 1H), 6.99-7.03 (m, 1H), 4.37-4.41 (m, 1H), 4.18-4.23 (m, 1H), 3.86-3.91 (m, 1H), 3.16-3.20 (m, 2H); Anal. Calcd for C25H22N4O.2TFA.H2O: C, 49.35; H, 3.61; N, 7.43; F, 22.67. Found: C, 49.04; H, 3.55; N, 7.42; F, 22.28.

Provenance & Evidence