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

HRID 434248

반응식

HRID 434248 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b75d6bb07b5d44b78dc473aa5b9c6e82
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06670473B2

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