HRID1436730

反应详情

EQUATION

反应方程式

HRID 1436730 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add powdered Zn (1.56 g, 24 mmol) portionwise at 0-5° C. to a stirred suspension of the (2S,3S)-2-dibenzylamino-4-nitro-1-phenyloct-7-en-3-ol mixture (2.7 g, 6 mmol) in a mixture of ethanol (20 mL) and concentrated HCl (20 mL). Stir for 1 h. Filter the reaction mixture and concentrate the filtrate under reduced pressure. Dilute residue with water and add concentrated ammonium hydroxide. Extract with dichloromethane. Wash the organic layer with water, dry (magnesium sulfate), and concentrate under reduced pressure to give the mixture of amines (1.5 g, 60%).

WORKUP

后处理

  1. filtrationFilter the reaction mixture
  2. concentrationconcentrate the filtrate under reduced pressure
  3. additionDilute residue with water and add concentrated ammonium hydroxide
  4. extractionExtract with dichloromethane
  5. washWash the organic layer with water
  6. dry with materialdry (magnesium sulfate)
  7. concentrationconcentrate under reduced pressure
  8. customto give