HRID1874608

反应详情

EQUATION

反应方程式

HRID 1874608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-{3-[(2-amino[1,2,4]triazolo[1,5-a]pyridin-6-yl)oxy]-4-methylphenyl}-3-(1-cyano-1-methylethyl)benzamide (200 mg, 0.469 mmol) in pyridine (5 mL) was added pyridine-3-carbonyl hydrochloride (212 mg, 1.19 mmol), and the mixture was stirred at room temperature for 3 hr. A saturated aqueous sodium hydrogen carbonate solution (20 mL) was added to the reaction mixture, and the mixture was extracted with ethyl acetate (20 mL, 5 mL). The combined organic layer was washed with saturated brine (5 mL) and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. Ethyl acetate was added to the obtained residue. The obtained precipitate was collected by filtration and dried to give the title compound (245 mg, 97%) as a colorless powder.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate (20 mL, 5 mL)
  2. washThe combined organic layer was washed with saturated brine (5 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationThe insoluble material was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionEthyl acetate was added to the obtained residue
  7. filtrationThe obtained precipitate was collected by filtration
  8. customdried