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
A solution of N-(1-(5-chlorobenzo[d][1,3]dioxol-7-yl)ethyl)-2-(methylsulfonyl)-5-(piperazin-1-yl)benzenamine (15.0 mg, 0.03 mmol) in anhydrous dichloromethane (0.5 mL) was cooled to 0° C. and HCl (34 μL of a 1M solution in diethyl ether, 0.03 mmol) were added. The mixture was allowed to stir for 30 min. The solvent was removed by rotary evaporation and co-evaporated with hexanes to precipitate the salt. After removal of solvent by rotary evaporation the desired product was collected (16 mg, 99%). 1H NMR (400 MHz, CD3OD): δ 7.55 (d, 1H), 6.92 (d, 1H), 6.78 (d, 1H), 6.41 (dd, 1H), 6.06 (m 1H), 5.99 (s, 1H), 4.69 (m, 1H), 3.44 (m, 4H), 3.26 (m, 4H), 3.06 (s, 3H), 1.59 (d, 3H); MS (ESI) m/z: 438.2.0 (M++1).
WORKUP
后处理
- customThe solvent was removed by rotary evaporation
- customto precipitate the salt
- customAfter removal of solvent
- customby rotary evaporation the desired product
- customwas collected (16 mg, 99%)