Trifluoroacetic acid methylene chloride → HCID 117728680, compound

Participants

Reaction Steps

A solution of compound 41g (0.20 g, 0.36 mmol) in TFA/CH2Cl2 (1:3, 3 mL) was stirred at rt for 2 h, and concentrated under reduced pressure. The resulting mixture was diluted with 10 mL of water. The solids formed were collected by filtration and washed with Et2O (2×30 mL). The crude solid product was then purified by re-crystallization from CH2Cl2:Et2O (1:10) to obtain the title compound 25 as a yellow solid. 1H-NMR (300 MHz, DMSO-d6) δ (ppm): 8.48 (d, J=8.4 Hz, 1H), 8.24 (d, J=5.7 Hz, 1H), 8.06-8.03 (m, 2H), 7.87-7.80 (m, 2H), 7.70-7.65 (m, 1H), 6.41 (d, J=6.0 Hz, 1H), 4.19 (s, 2H), 4.08-3.95 (m, 4H), 3.82-3.64 (m, 7H), 3.42-3.29 (m, 2H), 2.70-2.57 (m, 2H), 2.23-2.19 (m, 2H). Mass Spectrum (LCMS, ESI pos.): Calcd. for C28H28N6O3: 497.2 (M+H). Found: 497.2.

Provenance & Evidence