Reaktion #51480

Reaktionsgleichung

N-methyl-β-alaninenitrile

piperonyl chloride

→

N-(1,3-benzodioxol-5-ylmethyl)-N-methyl-1,3-propanediamine

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe solvent was removed in vacuo
2. 2
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2
3. 3
   Waschenwashed with aqueous carbonate
4. 4
   Trocknendried (MgSO4)
5. 5
   Sonstigethe solvent was removed in vacuo
6. 6
   workup.DISSOLUTIONThe residue was dissolved in methanol saturated with ammonia (600 mL) and Raney nickel (10 g)
7. 7
   workup.ADDITIONwas added
8. 8
   workup.STIRRINGAfter shaking under an atmosphere of hydrogen at 20 psi for 6 h
9. 9
   Filtrationthe reaction was filtered through celite
10. 10
    Sonstigethe solvent was removed in vacuo

Vorschrift

To N-methyl-β-alaninenitrile (50 g, mmol in acetonitrile was added piperonyl chloride (50 g, mmol). After stirring for 18 h, the solvent was removed in vacuo. The residue was dissolved in CH2Cl2, washed with aqueous carbonate, dried (MgSO4), and the solvent was removed in vacuo. The residue was dissolved in methanol saturated with ammonia (600 mL) and Raney nickel (10 g) was added. After shaking under an atmosphere of hydrogen at 20 psi for 6 h, the reaction was filtered through celite and the solvent was removed in vacuo to give 65 g of N-(1,3-benzodioxol-5-ylmethyl)-N-methyl-1,3-propanediamine.

Quelle