反应详情

A solution of N-(4-(2-(1-methylpyrrolidin-2-yl)ethyl)-3,4-dihydro-2H-benzo[b][1,4]thiazin-7-yl)thiophene-2-carboximidamide (0.48 g, 1.242 mmol) in dry ethanol (10 mL) was treated with hydrochloric acid (1M in ether; 6.21 mL, 6.21 mmol) and stirred for half an hour. The precipitate was collected and rinsed with ether. The precipitate was dissolved in methanol and concentrated to give a yellow-orange crystalline solid (0.57 g, 100%). 1H-NMR (DMSO-d6) δ 11.22 (brs, 1H), 11.17 (brs, 1H), 9.68 (brs, 1H), 8.72 (brs, 1H), 8.15-8.13 (m, 2H), 7.37-7.34 (m, 1H), 7.05-6.99 (m, 2H), 6.91 (brd, J=8.7 Hz, 1H), 3.66-3.64 (m, 2H), 3.55-3.41 (m, 3H), 3.38-3.22 (m, 1H), 3.12-3.09 (m, 2H), 3.00-2.97 (m, 1H), 2.76 (d, J=4.8 Hz, 3H), 2.32-2.18 (m, 2H), 1.99-1.86 (m, 3H), 1.77-1.71 (m, 1H); ESI-MS (m/z, %): 387 (MH+, free base, 100), 194 (19); ESI-HRMS calculated for C20H27N4S2 (MH+, free base): 387.1671, observed: 387.1654; HPLC purity: 97% by area.

1. customThe precipitate was collected
2. washrinsed with ether
3. dissolutionThe precipitate was dissolved in methanol
4. concentrationconcentrated