Fumaric Acid → HCID 67069975, compound

Participants

Reaction Steps

The product of Example 30B (200 mg, 0.625 mmol) was treated with fumaric acid (Aldrich, 73 mg, 0.63 mmol) in EtOAc/MeOH (v.10:1, 10 mL) at ambient temperature for 10 hours to give title compound (240.2 mg, 85%). 1H NMR (300 MHz, MeOH-D4) δ 1.87-2.22 (m, 3H), 2.31-2.45 (m, 1H), 2.60-2.67 (m, 1H), 3.30-3.50 (m, 5H), 3.89-4.00 (m, 1H), 5.49-5.57 (m, 1H), 6.57 (d, J=3.1 Hz, 1H), 6.68 (s, 2H), 7.28-7.35 (m, 2H), 7.52 (d, J=8.5 Hz, 1H), 7.74 (dd, J=8.6, 1.9 Hz, 1H), 8.11-8.19 (m, J=9.5 Hz, 2H) ppm. MS (DCI/NH3) m/z 321 (M+H)+. Anal. Calculated for C19H20N4O.1.0 C4O4H4.0.50 H2O: C, 62.01; H, 5.66; N, 12.58. Found: C, 61.79; H, 5.46; N, 12.43.

Provenance & Evidence