Reacción #51480

Ecuación de reacción

N-methyl-β-alaninenitrile

piperonyl chloride

→

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

Disolventes

acetonitrile

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrothe solvent was removed in vacuo
2. 2
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2
3. 3
   Lavadowashed with aqueous carbonate
4. 4
   Secadodried (MgSO4)
5. 5
   Otrothe 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
   Filtraciónthe reaction was filtered through celite
10. 10
    Otrothe solvent was removed in vacuo

Procedimiento

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.

Fuente