Fumaric Acid → HCID 86584382, compound

Participants

Reaction Steps

The product of Example 64C (90.0 mg, 0.302 mmol) in 20% CH3OH in diethyl ether (10 mL) was treated with a solution of fumaric acid (35.0 mg, 0.302 mmol) in 10% CH3OH in diethyl ether (5 mL). The mixture was stirred for 20 hours and the precipitate was isolated via filtration to provide the title compound (91.3 mg, 0.211 mmol, 70% yield). 1H NMR (CH3OH-d4, 300 MHz) δ 2.05 (in 1H), 2.35 (m, 1H), 3.32 (m, 5H), 3.45 (m, 2H), 3.84 (dd, J=11.5, 1.2 Hz, 1H), 4.39 (m, 1H), 4.57 (s, 2H), 6.67 (s, 2H), 7.33 (d, J=3.1 Hz, 1H), 7.72 (d, J=3.1 Hz, 1H); MS (DCI/NH3) m/z 299 (M+H−C4H4O4)+; Anal. calculated for C12H16BrN3O.C4H4O4.H2O: C, 44.46; H, 5.13; N, 9.72. Found: C, 44.39; H, 4.79; N, 9.66.

Provenance & Evidence