HRID1068054

反应详情

EQUATION

反应方程式

HRID 1068054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionThe free amine is extracted with dichloromethane (2×25 mL)
  2. washwashed with brine (5 mL)
  3. dry with materialdried with Na2SO4
  4. concentrationThe solution is concentrated in vacuo
  5. customto afford 1.48 g of a clear, colorless oil which
  6. temperatureto cool to room temperature
  7. customthe resulting solid is recrystallized in ethyl acetate