HRID2095942

反应详情

EQUATION

反应方程式

HRID 2095942 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a solution of N-[6-(4-amino-2-fluorophenoxy)imidazo[1,2-a]pyridin-2-yl]cyclopropanecarboxamide (90 mg, 0.276 mmol) and 1-(4-fluorophenyl)-2-oxo-6-(trifluoromethyl)-1,2-dihydropyridine-3-carboxylic acid (100 mg, 0.331 mmol) in N,N-dimethylformamide (2 mL) were added N,N-diisopropylethylamine (95 μL, 0.552 mmol) and HATU (126 mg, 0.331 mmol), and the mixture was stirred at room temperature for 6 hr. Ethyl acetate, tetrahydrofuran and saturated aqueous sodium hydrogen carbonate solution were added to the reaction mixture, and the mixture was extracted 3 times with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated under reduced pressure. The obtained residue was washed with ethyl acetate and collected by filtration. The obtained slightly yellow solid was suspended in ethanol (3 mL), and the mixture was stirred at 70° C. for 17 hr. The suspension was collected by filtration and washed with ethanol to give the title compound (32.7 mg, 19%) as a slightly yellow solid.

WORKUP

后处理

  1. extractionthe mixture was extracted 3 times with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customthe solvent was evaporated under reduced pressure
  6. washThe obtained residue was washed with ethyl acetate
  7. filtrationcollected by filtration
  8. customThe obtained slightly yellow solid
  9. stirringthe mixture was stirred at 70° C. for 17 hr
  10. filtrationThe suspension was collected by filtration
  11. washwashed with ethanol