Fumaric Acid → HCID 69432362, compound

Participants

Reaction Steps

The product of Example 22B (284 mg, 0.96 mmol) in ethyl acetate:ethanol (1:1, 10 mL) was treated with fumaric acid (116 mg, 1.0 mmol) at ambient temperature for 10 hours. The title compound was obtained as a solid (351 mg, yield, 87%). 1H NMR (300 MHz, MeOH-d4) δ 1.78-2.13 (m, 3H), 2.22-2.38 (m, 1H), 2.48-2.55 (m, 1H), 3.12-3.39 (m, 5H), 3.71-3.83 (m, 1H), 5.31-5.39 (m, 1H), 6.67 (s, 1.8H), 6.76 (ddd, J=8.2, 2.1, 1.0 Hz, 1H), 6.90 (ddd, J=7.4, 1.7, 1.0 Hz, 1H) 6.94 (t, J=1.8 Hz, 1H), 7.21 (t, J=7.8 Hz, 1H), 8.79 (s, 2H) ppm. MS (DCl/NH3) m/z 297 (M+H)+. Anal. Calculated for C17H20N4O.1.0C4H4O4.0.25H2O: C, 60.49; H, 5.92; N, 13.44. Found: C, 60.49; H, 5.94; N, 13.35.

Provenance & Evidence