반응 #51480

반응 방정식

N-methyl-β-alaninenitrile

piperonyl chloride

→

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

용매

acetonitrile

반응 조건

후처리

1. 1
   기타the solvent was removed in vacuo
2. 2
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2
3. 3
   세척washed with aqueous carbonate
4. 4
   건조dried (MgSO4)
5. 5
   기타the 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
   여과the reaction was filtered through celite
10. 10
    기타the solvent was removed in vacuo

실험 절차

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.

출처