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Cesium carbonate → 5-Bromo-2-(4-methyl-piperazin-1-yl)-benzonitrile

HRID 1175171
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HRID 1175171 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5](F)=[C:6]([CH:9]=1)[C:7]#[N:8].C(=O)([O-])[O-].[Cs+].[Cs+].[CH3:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>CS(C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([N:21]2[CH2:22][CH2:23][N:18]([CH3:17])[CH2:19][CH2:20]2)=[C:6]([CH:9]=1)[C:7]#[N:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 531671-MethylpiperazineHCID 27249005-Bromo-2-fluorobenzonitrile

생성물 1

HCID 595583365-Bromo-2-(4-methyl-piperazin-1-yl)-benzonitrile

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

5-Bromo-2-fluorobenzonitrile (2.0 g, 10 mmol), Cesium carbonate (6.58 g, 20 mmol) and 1-methylpiperazine (1.35 ml, 12 mmol) in 100 ml DMSO are stirred at 120 C for 1 hour. The reaction is quenched by the addition of water and extracted with ethyl acetate. The organic phases are dried and the solvent evaporated. The product obtained is considered pure enough for the next synthesis steps. LC-MS (m/z, ES+): 280 (MH+), Retention time: 1.03 mins (LC-MS method 8)

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후처리

  1. customThe reaction is quenched by the addition of water
  2. extractionextracted with ethyl acetate
  3. customThe organic phases are dried
  4. customthe solvent evaporated
  5. customThe product obtained
  6. customis considered pure enough for the next synthesis steps

출처 및 근거

ORD 기록
ord-56daa61b81b24ba49faa38c4e0050ab8
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07838674B2

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