HRID488499

反应详情

EQUATION

反应方程式

HRID 488499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-[3-(3,4-dichloro-phenyl)propyl]phenylamine (0.94 g, 3.3 mmol), 2-fluoro-4-methoxy-5-nitro-benzoic acid methyl ester (0.75 g, 3.3 mmol), and Et3N (0.46 mL) in CH3CN (30 mL) was heated to reflux for 120 hours. The reaction mixture was cooled to room temperature, diluted with CH2Cl2 and washed with saturated NaHCO3. The organic layer was dried (Na2SO4) and concentrated to give a solid. Recrystallization with MeOH yielded 0.67 g (1.37 mmol, 42%) of the desired product.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 120 hours
  3. washwashed with saturated NaHCO3
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. concentrationconcentrated
  6. customto give a solid
  7. customRecrystallization with MeOH