反応 #51480

反応方程式

N-methyl-β-alaninenitrile

piperonyl chloride

→

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

溶媒

acetonitrile

反応条件

後処理

1. 1
   その他the solvent was removed in vacuo
2. 2
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2
3. 3
   洗浄washed with aqueous carbonate
4. 4
   乾燥dried (MgSO4)
5. 5
   その他the 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
   ろ過the reaction was filtered through celite
10. 10
    その他the solvent was removed in vacuo

実験手順

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.

出典