HRID2367386

反应详情

EQUATION

反应方程式

HRID 2367386 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2-{4-[3-(methyloxy)phenyl]-1H-imidazol-2-yl}morpholine (1.5 g, 5.07 mmol) and 4,6-dichloro-2-pyrimidinamine (0.832 g, 5.07 mmol) in ethanol (100 mL) was added Hunig's base (4.5 mL, 25.4 mmol), and the reaction mixture was stirred overnight at reflux. Water (150 mL) was added, and the resulting mixture was extracted with EtOAc (3×100 mL). The organic was dried (Na2SO4), filtered, and concentrated. Purification by silica gel chromatography, eluting with EtOAc in PE from 50% to 80% afforded the title compound (830 mg) as a brown solid. LC-MS (ES) m/z=387 [M+H]+.

WORKUP

后处理

  1. temperatureat reflux
  2. extractionthe resulting mixture was extracted with EtOAc (3×100 mL)
  3. dry with materialThe organic was dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by silica gel chromatography
  7. washeluting with EtOAc in PE from 50% to 80%