HRID2095956

反应详情

EQUATION

反应方程式

HRID 2095956 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution (90 mL) of N-[4-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-a]pyridin-6-yl}oxy)phenyl]-1-(4-fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxamide (400 mg, 0.744 mmol) in tetrahydrofuran was added benzenesulfonic acid monohydrate (197 mg, 1.12 mmol) at 80° C. The mixture was filtered, and the filtrate was gradually cooled to room temperature. The solution at room temperature was distilled off at 110° C. to evaporate tetrahydrofuran to about half, and gradually cooled again to room temperature. The precipitate was collected by filtration, and the solid was washed with tetrahydrofuran and dried to give the title compound (309 mg, 58%) as a white solid.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. distillationThe solution at room temperature was distilled off at 110° C.
  3. customto evaporate tetrahydrofuran to about half
  4. temperaturegradually cooled again to room temperature
  5. filtrationThe precipitate was collected by filtration
  6. washthe solid was washed with tetrahydrofuran
  7. customdried