Dimethyl Sulfoxide → 1-(3-Cyanophenyl)piperazine
반응식
F[C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[C:5]#[N:6].[NH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.CS(C)=O>O>[C:5]([C:4]1[CH:3]=[C:2]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[CH:9]=[CH:8][CH:7]=1)#[N:6]참가 물질
5
반응 조건
- 온도
- 100 °C
실험 절차
A mixture of 3-fluorobenzonitrile (3.0 g, 25 mmol), piperazine (11.8 g, 137 mmol) and dimethylsulphoxide (20 ml) is heated at 100° C. for 48 hours under an atmosphere of nitrogen. The reaction mixture is then cooled, poured into water (200 ml) and the resultant precipitate collected. This solid is chromatographed on silica gel (dichloromethane) to give the title compound as a white solid (6.7 g). 1H NMR (DMSO, 500 MHz) δ7.15-7.40 (m, 4H), 3.28 (m, 3H), 3.12 (m, 1H), 2.80 (m, 1H), 2.59 (m, 3H).
후처리
- temperatureThe reaction mixture is then cooled
- customthe resultant precipitate collected
- customThis solid is chromatographed on silica gel (dichloromethane)
출처 및 근거
- ORD 기록
- ord-54a39dc3799e48f296756f3420669cff
- 출처 데이터셋
- uspto-grants-2011_05
- 특허 번호
- US07947684B2
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