Piperazine → 4-Fluoro-2-(piperazin-1-yl)benzonitrile

HRID 1416286

반응식

HRID 1416286 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.F[C:8]1[CH:15]=[C:14]([F:16])[CH:13]=[CH:12][C:9]=1[C:10]#[N:11]>CN(C)C(=O)C>[C:10]([C:9]1[CH:8]=[CH:15][C:14]([F:16])=[CH:13][C:12]=1[N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)#[N:11]

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 775452,4-Difluorobenzonitrile

생성물 1

HCID 193671084-Fluoro-2-(piperazin-1-yl)benzonitrile

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
122 °C

실험 절차

A mixture of piperazine (Aldrich; 3.99 g), 2,4-difluorobenzonitrile, and N,N-dimethylacetamide (20 mL) is stirred for 1.5 h at 122° C. After cooling, the mixture is partitioned between dichloromethane and satd. aq. sodium bicarbonate. The organic layers are dried over magnesium sulfate and concentrated. The residue is chromatographed on silica gel and the appropriate fractions are combined and concentrated to give 1.44 g of 1-(2-cyano-5-fluorophenyl)piperazine; 1H NMR (CDCl3) δ3.01, 3.30, 6.56, 6.63, 7.40.

후처리

  1. temperatureAfter cooling
  2. customthe mixture is partitioned between dichloromethane
  3. dry with materialThe organic layers are dried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue is chromatographed on silica gel
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5980976b2f5f4071b3a4e96b7f854466
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05912246

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