反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
[1-(5-Chloro-2,3-dimethoxy-phenyl)-ethyl]-(2-methanesulfonyl-5-piperazin-1-yl-phenyl)-amine (10 mg, 0.022 mmol) was dissolved in dichloromethane (1.5 mL) and ether (1.5 mL). The solution was cooled in a bath with dry ice and methanol. Hydrochloric acid (0.5 mL, 2.0 M in ether) was added slowly. The mixture was warmed to room temperature. The solvents were concentrated down in vacuo and co-evaporated with diethyl ether gave [1-(5-chloro-2,3-dimethoxy-phenyl)-ethyl]-(2-methanesulfonyl-5-piperazin-1-yl-phenyl)-amine hydrochloride salt as a white solid (10.6 mg): 1H NMR (400 MHz, CD3OD): 1H NMR (400 MHz, CD3OD): δ 7.51 (d, 1H), 6.92 (m, 2H), 6.37 (dd, 1H), 6.09 (d, 1H), 4.93 (m, 1H), 3.90 (s, 3H), 3.86 (s, 3H), 3.48 (m, 4H), 3.24 (m, 4H), 3.05 (s, 3H), 1.49 (d, 3H). MS (ESI) m/z: Calculated: 453.98 free base; Observed: 454.4 (M+H+); 476.4 (M+Na+); 930.8 (2M+Na+). Salt: Mol. Wt.: 490.44 (C21H29Cl2N3O4S).
WORKUP
后处理
- concentrationThe solvents were concentrated down in vacuo and co-evaporated with diethyl ether