Piperazine → N,N'-bis[(5,6,7-trimethoxynaphthalen-2-yl)methyl]piperazine

HRID 987412ノート

反応式

HRID 987412 の反応式
Cl[CH2:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][C:7]([O:17][CH3:18])=[C:8]([O:15][CH3:16])[C:9]=2[O:13][CH3:14])[CH:4]=1.[NH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.[C:25](=[O:28])([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:14][O:13][C:9]1[C:8]([O:15][CH3:16])=[C:7]([O:17][CH3:18])[CH:6]=[C:5]2[C:10]=1[CH:11]=[CH:12][C:3]([CH2:2][N:19]1[CH2:24][CH2:23][N:22]([CH2:2][C:3]3[CH:12]=[CH:11][C:10]4[C:5](=[CH:6][C:7]([O:28][CH3:25])=[C:8]([O:15][CH3:16])[C:9]=4[O:13][CH3:14])[CH:4]=3)[CH2:21][CH2:20]1)=[CH:4]2

参加物

5

反応物 3

HCID 4837PiperazineHCID 11430Potassium CarbonateHCID 218916422-Chloromethyl-5,6,7-trimethoxynaphthalene

生成物 1

HCID 12108580N,N'-bis[(5,6,7-trimethoxynaphthalen-2-yl)methyl]piperazine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-Chloromethyl-5,6,7-trimethoxynaphthalene (418 mg) and piperazine (63 mg) were dissolved in DMF (10 mL), potassium carbonate (207 mL) was added to the solution, and the mixture was stirred at room temperature for 5 hours. After concentrating the reaction mixture under reduced pressure, chloroform was added to the residue, and the mixture was washed with water and saturated brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (chloroform:methanol=40:1) to obtain the title compound as a free base.

後処理

  1. concentrationAfter concentrating the reaction mixture under reduced pressure, chloroform
  2. additionwas added to the residue
  3. washthe mixture was washed with water and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel (chloroform:methanol=40:1)

出典と根拠

ORDレコード
ord-49a2a0c6e99e42748b7126b071638a59
出典データセット
uspto-grants-2003_10
特許番号
US06632810B2

反応ノート

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