反应详情

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.

1. customthe solvent was removed in vacuo
2. dissolutionThe residue was dissolved in CH2Cl2
3. washwashed with aqueous carbonate
4. dry with materialdried (MgSO4)
5. customthe solvent was removed in vacuo
6. dissolutionThe residue was dissolved in methanol saturated with ammonia (600 mL) and Raney nickel (10 g)
7. additionwas added
8. stirringAfter shaking under an atmosphere of hydrogen at 20 psi for 6 h
9. filtrationthe reaction was filtered through celite
10. customthe solvent was removed in vacuo