HRID1043955

反应详情

EQUATION

反应方程式

HRID 1043955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of ethyl 5-[4-(6-isopropyloxy-2,4-dimethylpyridin-3-yl)-2-nitrophenyl]-1-[(S)-tetrahydrofuran-3-yl]-1H-pyrazole-4-carboxylate (65.1 mg) in acetic acid (1.5 mL)-water (0.15 mL) was stirred at 80° C. for 15 minutes. Iron powder (45.1 mg) was added to the solution, and the mixture was stirred at the same temperature for two hours in a nitrogen atmosphere. The reaction mixture was returned to room temperature, and ethyl acetate (5 mL) was added to the reaction mixture. The insoluble matter was removed by filtration through Celite™. The filtrate was concentrated under reduced pressure. A solution of the residue in ethyl acetate was washed with a saturated aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure. The residue was suspended and triturated by adding MTBE. The precipitated solid was collected by filtration to give the title compound (35.1 mg).

WORKUP

后处理

  1. customwas returned to room temperature
  2. customThe insoluble matter was removed by filtration through Celite™
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. washA solution of the residue in ethyl acetate was washed with a saturated aqueous sodium bicarbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customtriturated
  9. additionby adding MTBE
  10. filtrationThe precipitated solid was collected by filtration