Piperazine → N,N'-bis[[2-(3,4,5-Trimethoxyphenyl)thiazol-4-yl]methyl]piperazine

HRID 992987노트

반응식

HRID 992987 반응식
Cl[CH2:2][C:3]1[N:4]=[C:5]([C:8]2[CH:13]=[C:12]([O:14][CH3:15])[C:11]([O:16][CH3:17])=[C:10]([O:18][CH3:19])[CH:9]=2)[S:6][CH:7]=1.[NH:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1.[C:26](=[O:29])([O-])[O-].[K+].[K+].[I-].[K+]>CN(C=O)C>[CH3:19][O:18][C:10]1[CH:9]=[C:8]([C:5]2[S:6][CH:7]=[C:3]([CH2:2][N:20]3[CH2:25][CH2:24][N:23]([CH2:2][C:3]4[N:4]=[C:5]([C:8]5[CH:9]=[C:10]([O:18][CH3:19])[C:11]([O:16][CH3:17])=[C:12]([O:29][CH3:26])[CH:13]=5)[S:6][CH:7]=4)[CH2:22][CH2:21]3)[N:4]=2)[CH:13]=[C:12]([O:14][CH3:15])[C:11]=1[O:16][CH3:17]

참가 물질

6

반응물 4

HCID 4837PiperazineHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 12010380HCID 12010380, 화합물

생성물 1

HCID 10232655N,N'-bis[[2-(3,4,5-Trimethoxyphenyl)thiazol-4-yl]methyl]piperazine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-Chloromethyl-2-(3,4,5-trimethoxyphenyl)thiazole (240 mg) and piperazine (34 mg) were dissolved in DMF (3 mL), potassium carbonate (166 mL) and potassium iodide (166 mg) were 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-e975b50b4bea4daa989b41c5dc76fad7
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06472386B1

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