p-Toluenesulfonic acid monohydrate → HCID 86760919, compound

Participants

Reaction Steps

p-Toluenesulfonic acid monohydrate (78 mg, 0.41 mmol) and the product of Example 7A (0.15 g, 0.41 mmol) were processed as in Example 1E. Recrystallization with CH3OH and EtOAc provided 25 mg of the title compound (0.050 mmol, 12% yield). 1H NMR (MeOH-d4, 300 MHz) δ 1.33 (s, 12H), 1.54 (m, 3H), 1.91 (br q, J=7.1 Hz, 2H), 2.03 (m, 2H), 2.15 (s, 1H), 2.81 (s, 3H), 2.93 (m, 2H), 3.26 (m, 1H), 3.45 (m, 2H), 4.34 (t, J=7.1 Hz, 2H), 6.70 (s, 2H), 7.21 (dd, J=7.8, 1.0 Hz, 1H), 7.27 (dd, J=7.1, 1.4 Hz, 1H), 7.49 (br d, J=8.1 Hz, 1H), 8.09 (s, 1H), 8.25 (br d, J=7.1 Hz, 1H); MS (DCI/NH3) m/z 367 (M+H)+; Anal. Calculated for C24H34N2O.C4H4O4.0.5CH4O: C, 68.65; H, 8.09; N, 5.62. Found: C, 68.68; H, 8.49; N, 5.82.

Provenance & Evidence