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1-Methylpiperazine → 2-Methyl-6'-(4-methyl-piperazin-1-yl)-[3,4']bipyridinyl-3'-carboxylic acid (3,5-bis-trifluoromethyl-benzyl)-methyl-amide

HRID 347688
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인쇄 미리보기

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HRID 347688 반응식
[F:1][C:2]([F:33])([F:32])[C:3]1[CH:4]=[C:5]([CH:25]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:27]=1)[CH2:6][N:7]([CH3:24])[C:8]([C:10]1[CH:11]=[N:12][C:13](Cl)=[CH:14][C:15]=1[C:16]1[C:17]([CH3:22])=[N:18][CH:19]=[CH:20][CH:21]=1)=[O:9].[CH3:34][N:35]1[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]1>ClCCl>[F:1][C:2]([F:33])([F:32])[C:3]1[CH:4]=[C:5]([CH:25]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:27]=1)[CH2:6][N:7]([CH3:24])[C:8]([C:10]1[CH:11]=[N:12][C:13]([N:38]2[CH2:39][CH2:40][N:35]([CH3:34])[CH2:36][CH2:37]2)=[CH:14][C:15]=1[C:16]1[C:17]([CH3:22])=[N:18][CH:19]=[CH:20][CH:21]=1)=[O:9]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 586945956'-Chloro-2-methyl-[3,4']bipyridinyl-3'-carboxylic acid (3,5-bis-trifluoromethyl-benzyl)-methyl-amide

생성물 1

HCID 115196362-Methyl-6'-(4-methyl-piperazin-1-yl)-[3,4']bipyridinyl-3'-carboxylic acid (3,5-bis-trifluoromethyl-benzyl)-methyl-amide수율 70.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
120 °C

실험 절차

A mixture of 0.21 g (0.44 mmol) 6′-chloro-2-methyl-[3,4′]bipyridinyl-3′-carboxylic acid (3,5-bis-trifluoromethyl-benzyl)-methyl-amide and 1.0 ml (9.0 mmol) 1-methylpiperazine was heated at 120° C. for 2 h. After cooling to room temperature the mixture was diluted with dichloromethane and washed with water. The aqueous layer was extracted with dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated in vacuo to give 0.25 g of crude product. Flash chromatography gave 0.17 g (70%) of the title compound. MS m/e (%): 552 (M+H+, 100)

후처리

  1. temperatureAfter cooling to room temperature the mixture
  2. washwashed with water
  3. extractionThe aqueous layer was extracted with dichloromethane
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto give 0.25 g of crude product

출처 및 근거

ORD 기록
ord-0ea5e34bdcf54b28b7aafa3b3cb614d2
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07176205B2

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