Hydrochloric Acid → HCID 178490669, compound

Participants

Reaction Steps

To a solution of Example 29B (140 mg, 0.28 mmol.) in methanol (2 mL) was added hydrogen chloride in dioxane (0.5 mL, 2.000 mmol) and stirred for 12 hr. The solvent was removed under reduced pressure and the residue recrystallized from methanol:diethyl ether to provide the title compound as a hydrogen chloride salt. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.33 (s, 9 H) 1.68-1.79 (m, 1 H) 1.87-2.01 (m, 2 H) 2.03-2.12 (m, 1 H) 3.14-3.28 (m, 2 H) 3.81 (s, 3 H) 3.93-4.06 (m, 1 H) 4.47 (d, J=6.44 Hz, 2 H) 7.14 (d, J=9.16 Hz, 1 H) 7.45-7.50 (m, 2 H) 7.63 (d, J=2.71 Hz, 1 H) 9.29 (d, J=4.41 Hz, 2 H); MS (DCI) m/z 408 (M+H)+. Anal. calcd for C20H26ClN3O2S.2HCl.1.0H2O: C, 48.15; H, 6.06; N, 8.42. Found: C, 48.00; H, 6.04; N, 8.27.

Provenance & Evidence