HRID2426052

反应详情

EQUATION

反应方程式

HRID 2426052 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customThe solvent was removed by rotary evaporation
  2. customto precipitate the salt
  3. customAfter removal of solvent
  4. customby rotary evaporation the desired product
  5. customwas collected (16 mg, 99%)