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-(Dimethylamino)ethyl)-3,4-dihydro-2H-benzo[b][1,4]thiazin-7-yl)furan-2-carboximidamide (0.166 g, 0.504 mmol) was dissolved in MeOH (2 mL). 1M HCl in ether (2.52 mL, 2.52 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 light yellow solid (0.18 g, 93%). 1H NMR (DMSO-d6) δ 11.36 (s, 1H), 11.25 (brs, 1H), 9.68 (s, 1H), 8.69 (s, 1H), 8.23 (s, 1H), 7.91 (d, J=2.7 Hz, 1H), 7.07-6.96 (m, 3H), 6.90 (d, J=1.8 Hz, 1H), 3.82-3.77 (m, 2H), 3.67-3.63 (m, 2H), 3.25-3.22 (m, 2H), 3.12-3.09 (m, 2H), 2.80 (s, 3H), 2.78 (s, 3H); ESI-MS (m/z, %): 333, 331 (MH+, free base, 100), 260, 262 (57); HRMS calculated for C17H23N4OS (MH+, free base): calculated: 331.1587, observed: 331.1589; HPLC purity: 98% by area.
WORKUP
后处理
- concentrationThe mixture was concentrated