p-Toluenesulfonic acid monohydrate → HCID 86599901, compound

Participants

Reaction Steps

The product of Example 1C (50 mg, 0.12 mmol) was dissolved in ethyl acetate (5 mL) and ethanol (0.2 mL), then p-toluenesulfonic acid monohydrate (46 mg, 0.24 mmol; Aldrich) was added. After stirring the mixture for 16 hours, the resulting solid was collected by filtration to afford the title compound (68 mg, 0.09 mmol; 74%): 1H NMR (300 MHz, methanol-d4): δ 7.68 (4H, d, J=8 Hz), 7.54 (2H, d, J=8 Hz), 7.27-7.14 (8H, m), 4.46 (2H, dd, J=11, 3 Hz), 4.27 (2H, dd, J=11, 7 Hz), 3.88 (2H, m), 3.73 (2H, m), 3.35-3.19 (4H, m), 3.07 (6H, s), 2.48-1.97 (12H, m). MS (DCI/NH3): m/z 407 (M+1)+. Anal. Calcd. for C25H30N2O3.2C7H8O3S.H2O: C, 60.92; H, 6.29; N, 3.64. Found: C, 61.02; H, 6.25; N, 3.57.

Provenance & Evidence