HRID2271556
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureThe solution was cooled to room temperature
- concentrationconcentrated
- customThe resultant residue was purified by preparative HPLC (C18 silica, 10-90% methanol/water with 0.05% TFA)
- washThe residue was eluted through an ion-exchange column (using methanol and 7 N methanol in ammonia)