HRID1932457

反应详情

EQUATION

反应方程式

HRID 1932457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl 3-[4-(5-nitropyridin-2-ylsulfanyl)phenyl]propionate (2.97 g, 9.33 mmol) in methanol (50 mL) were added sodium borohydride (0.590 g, 15.6 mmol) and 10% palladium-carbon (1.80 g), and the resulting solution was stirred for 24 hours at room temperature under a hydrogen atmosphere at atmospheric pressure. The reaction solution was filtered through Celite, and to the resulting filtrate was added concentrated hydrochloric acid (1.5 mL), and concentrated under reduced pressure. To the residue was added a saturated sodium bicarbonate solution, and extracted with ethyl acetate, and the ethyl acetate layer was washed with brine. The ethyl acetate layer was dried over anhydrous magnesium sulfate, and evaporated, to thereby yield 2.49 g of the title compound.

WORKUP

后处理

  1. filtrationThe reaction solution was filtered through Celite
  2. additionto the resulting filtrate was added concentrated hydrochloric acid (1.5 mL)
  3. concentrationconcentrated under reduced pressure
  4. additionTo the residue was added a saturated sodium bicarbonate solution
  5. extractionextracted with ethyl acetate
  6. washthe ethyl acetate layer was washed with brine
  7. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
  8. customevaporated