Fumaric Acid → HCID 67070277, compound

Participants

Reaction Steps

The product of Example 4C (50 mg, 0.25 mmol) was treated with fumaric acid (29 mg, 0.25 mmol) in EtOAc/EtOH (v. 1:1, 4 mL) at ambient temperature for 10 h. The title compound was obtained as solid (56.9 mg, yield, 52%). 1H NMR (300 MHz, CD3OD) δ 1.78–2.16 (m, 3H), 2.25–2.39 (m, 1H), 2.46–2.54 (m, 1H), 3.14–3.45 (m, 5H), 3.69–3.81 (m, 1H), 4.80–4.89 (m, 1H), 6.46 (dd, J=3.0, 1.0, 1H), 6.68 (s, 2.2H), 7.02 (dt, J=8.8, 2.5 Hz, 2H), 7.23 (d, J=3.1 Hz, 1H), 7.31 (dd, J=8.5, 2.0 Hz, 1H), 7.43 (dt, J=8.4, 0.8 Hz, 1H), 7.58 (dt, J=9.2, 2.6 Hz, 2H), 7.71 (dd, J=1.7, 1.0 Hz, 1H) ppm. MS (DCl/NH3): m/z 319 (M+H)+. Anal. Calculated for C21H22N2O.1.14C4H4O4: C, 68.11; H, 5.94; N, 6.21. Found: C, 68.12; H, 6.04; N, 6.18.

Provenance & Evidence