Reaction #965606

ord-b854fd749a1a4bc8bd7bfa7179f2a690

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Procedure

Prepared from the product of Example 17A (81 mg, 0.33 mmol) and HCl-dioxane (160 μL, 0.66 mmol; Aldrich, 4.0 M) according to Method H: 1H NMR (300 MHz, methanol-D4) δ ppm 1.92 (d, J=12.2 Hz, 2H), 2.19 (s, 1H), 2.34 (d, J=13.2 Hz, 2H), 2.46 (s, 2H), 3.56 (s, 2H), 3.58-3.74 (m, 4H), 4.77 (t, J=3.2 Hz, 1H), 7.04 (dd, J=9.5, 0.7 Hz, 1H), 7.73 (dd, J=3.1, 0.7 Hz, 1H), 7.89 (dd, J=9.5, 2.7 Hz, 1H). MS (+ESI) m/z=246 (M+H)+. Anal. Calcd. for C14H19N3O.2HCl.0.5H2O: C, 51.38; H, 6.78; N, 12.84. Found: C, 51.06; H, 6.47; N, 12.68.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08987453B2uspto-grants-2015_03