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

HRID 720304노트

반응식

HRID 720304 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-7b47c8a656944c938b7dff0ac062ffa2
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07135473B2

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