HRID2271556

反应详情

EQUATION

反应方程式

HRID 2271556 的结构方程式

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A suspension of (trans-4-((6-bromo-3-(cyclopropanecarbonyl)quinolin-4-yl)amino)cyclohexyl)methyl methanesulfonate (175 mg, 0.36 mmol) in methylamine (2.0 M solution in THF, 4.0 mL, 8.0 mmol) in a sealed vessel was heated under microwave irradiation conditions to 120° C. for 2 h. The solution was cooled to room temperature and concentrated. The resultant residue was purified by preparative HPLC (C18 silica, 10-90% methanol/water with 0.05% TFA). The residue was eluted through an ion-exchange column (using methanol and 7 N methanol in ammonia) to obtain the desired product (42 mg, 28%) a white solid. ESI MS m/z 416 [C21H26BrN3O+H]+

WORKUP

后处理

  1. temperatureThe solution was cooled to room temperature
  2. concentrationconcentrated
  3. customThe resultant residue was purified by preparative HPLC (C18 silica, 10-90% methanol/water with 0.05% TFA)
  4. washThe residue was eluted through an ion-exchange column (using methanol and 7 N methanol in ammonia)