反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
N-(4-(2-(methylamino)ethyl)-3,4-dihydro-2H-benzo[b][1,4]thiazin-7-yl)furan-2-carboximidamide (0.4353 g, 1.376 mmol) was dissolved in MeOH (3 mL). 1M HCl in ether (6.88 mL, 6.88 mmol) was added to the solution at room temperature, and the reaction was stirred for 5 minutes under argon atmosphere. The mixture was concentrated to give a yellow solid (0.59 g, quantitative). 1H NMR (DMSO-d6) δ 11.31 (s, 1H), 9.58 (s, 1H), 9.30 (brs, 2H), 8.82 (s, 1H), 8.57 (s, 1H), 7.98 (s, 1H), 7.30 (d, J=1.2 Hz, 1H), 7.06-7.03 (m, 2H), 6.97 (dd, J=2.4, 8.7 Hz, 1H), 3.74-3.63 (m, 4H), 3.13-3.05 (m, 4H), 2.58-2.55 (m, 3H); ESI-MS (m/z, %): 319, 317 (MH+, free base, 100), 260 (98); HRMS calculated for C16H20N4OS (MH+, free base), calculated: 317.1430, observed: 317.1417; HPLC purity: 99% by area.
WORKUP
后处理
- concentrationThe mixture was concentrated
- customto give a yellow solid (0.59 g, quantitative)