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

HRID 23202
Notes
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Reaction equation

HRID 23202 reaction equation
[CH3:1][NH:2][CH2:3][CH2:4][C:5]#[N:6].[CH2:7](Cl)[C:8]1[CH:16]=[CH:15][C:14]2[O:13][CH2:12][O:11][C:10]=2[CH:9]=1>C(#N)C>[O:13]1[C:14]2[CH:15]=[CH:16][C:8]([CH2:7][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][NH2:6])=[CH:9][C:10]=2[O:11][CH2:12]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 69656Propanenitrile, 3-(methylamino)-HCID 887131,3-Benzodioxole, 5-(chloromethyl)-

Product 1

HCID 22488891N-(1,3-benzodioxol-5-ylmethyl)-N-methyl-1,3-propanediamine

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-d0d61cfbd0134a90a8798f2eab515344
Source dataset
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06849739B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes