Reaktion #2470535

ord-b40418d3d3c14790872c3254466e6f09

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGThe reaction mixture is stirred at room temperature for 15 hours
  2. 2
    Extraktionthe product is extracted with dichloromethane
  3. 3
    ExtraktionThe organic extract
  4. 4
    Waschenis washed with water
  5. 5
    Trocknendried over anhydrous sodium sulphate
  6. 6
    FiltrationAfter filtration
  7. 7
    Sonstigethe solvent is removed on a rotary evaporator
  8. 8
    TrocknenThe crude product is dried under high vacuum
  9. 9
    Sonstigeused without further purification in the next reaction
  10. 10
    SonstigeWhat is obtained

Vorschrift

1.34 g (3.581 mmol) of the product from Example 2A and 538 μl (3.581 mmol) of 2,4-dimethoxybenzylamine are dissolved in 40 ml of dichloroethane, and the mixture is stirred at room temperature for one hour. 1.52 g (7.162 mmol) of sodium triacetoxyborohydride and 820 μl (14.33 mmol) of glacial acetic acid are then added. The reaction mixture is stirred at room temperature for 15 hours. A saturated sodium bicarbonate solution is then added, and the product is extracted with dichloromethane. The organic extract is washed with water and dried over anhydrous sodium sulphate. After filtration, the solvent is removed on a rotary evaporator. The crude product is dried under high vacuum and used without further purification in the next reaction. What is obtained are 1.89 g of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08263624B2uspto-grants-2012_09