3-甲胺基丙腈 → N-(1,3-benzodioxol-5-ylmethyl)-N-methyl-1,3-propanediamine

HRID 434248

反应方程式

HRID 434248 反应方程式
[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

参与物

4

反应物 2

HCID 696563-甲胺基丙腈HCID 88713胡椒基氯

产物 1

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

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-b75d6bb07b5d44b78dc473aa5b9c6e82
来源数据集
uspto-grants-2003_12
专利号
US06670473B2

关联笔记

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