Trifluoroacetic acid methylene chloride → HCID 11456638, compound

Participants

Reaction Steps

Compound 6a (0.29 g, 0.06 mmol) and TFA/CH2Cl2 (1:1, 2 ml) containing H2O (40 μl) were stirred at room temperature for 1.5 hr. The solvent was removed under pressure and the residue stirred with DOWEX® 550A OH anion exchange resin (0.05 g, 0.17 mmol, washed with MeOH). The solution was decanted and evaporated. CHCl3 (5 ml) was added and the solid collected and dried under vacuum. Yield 0.02 g (90%). 1H NMR (DMSO): δ 10.49 (s, 1H, NH), 9.96 (s, 1H, NH), 8.13 (t, 1H, NH, J=6.0 Hz) 7.71 (bs, 2H, NH2), 7.40 (d, 1H, J=1.5 Hz), 7.28 (d, 1H, J=1.5 Hz), 7.18 (d, 1H, J=1.5 Hz) 7.15 (d, 1H, J=1.8 Hz), 7.04 (d, 1H, J=1.2 Hz), 6.98 (d, 1H J=1.5 Hz), 3.98 (s, 3H), 3.83 (s, 3H), 3.81 (s, 3H), 3.5-3.2 (m, 2H, CH2), 2.92 (m, 2H, CH2).

Provenance & Evidence