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

HRID 434248

反応式

HRID 434248 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

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.

後処理

  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

出典と根拠

ORDレコード
ord-b75d6bb07b5d44b78dc473aa5b9c6e82
出典データセット
uspto-grants-2003_12
特許番号
US06670473B2

関連ノート

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