HRID1062811

反应详情

EQUATION

反应方程式

HRID 1062811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(E)-N-[4-(1,3-benzodioxol-5-yl)-1-benzyl-3-methoxy-1H-pyrazol-5-yl]-2-phenyl-1-ethenesulfonamide (1.2 g) (Preparation 57) was dissolved in acetic acid (50 ml). Under an atmosphere of nitrogen, Pearlmann's catalyst (JM type 91, 200 mg) was added and the reaction was stirred for 24 h under 2 bars of hydrogen at 50C. The reaction mixture was filtered on a short pad of Celite® and concentrated under reduced pressure. To the oily residue was added water (dichloromethane (200 ml). The phases were separated, the organic phase washed with a 10% aqueous solution of sodium bicarbonate (2×100 ml). The aqueous phase was then extracted with dichloromethane (2×10 ml), the combined organic fractions were dried over sodium sulfate and concentrated under reduced pressure to yield the title compound as a colourless oil (0.96 g).

WORKUP

后处理

  1. additionUnder an atmosphere of nitrogen, Pearlmann's catalyst (JM type 91, 200 mg) was added
  2. filtrationThe reaction mixture was filtered on a short pad of Celite®
  3. concentrationconcentrated under reduced pressure
  4. additionTo the oily residue was added water (dichloromethane (200 ml)
  5. customThe phases were separated
  6. washthe organic phase washed with a 10% aqueous solution of sodium bicarbonate (2×100 ml)
  7. extractionThe aqueous phase was then extracted with dichloromethane (2×10 ml)
  8. dry with materialthe combined organic fractions were dried over sodium sulfate
  9. concentrationconcentrated under reduced pressure