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
CONDITIONS
反应条件
- 温度
- 190 °C
PROCEDURE
实验过程
4-Bromobenzylamine hydrochloride (2.22 g) is suspended in water (5 mL) and neutralized with 2N aqueous NaOH (5 mL). The free amine is extracted with dichloromethane (2×25 mL). The organic layers are combined, washed with brine (5 mL), and dried with Na2SO4. The solution is concentrated in vacuo to afford 1.48 g of a clear, colorless oil which is then combined with ethyl 1-(4-morpholinyl)-6-(4-morpholinylmethyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylate (0.48 g) from Preparation No. 56 and heated to 190° C. for 3 hours. The reaction mixture is allowed to cool to room temperature, and the resulting solid is recrystallized in ethyl acetate to afford 0.44 g of the title compound as a white solid.
WORKUP
后处理
- extractionThe free amine is extracted with dichloromethane (2×25 mL)
- washwashed with brine (5 mL)
- dry with materialdried with Na2SO4
- concentrationThe solution is concentrated in vacuo
- customto afford 1.48 g of a clear, colorless oil which
- temperatureto cool to room temperature
- customthe resulting solid is recrystallized in ethyl acetate