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

HRID 849493

반응식

HRID 849493 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) δ 3.01, 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-9ef007546ddc48d2936bb14ca1172ab3
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06013654

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