Piperazine → 4-Fluoro-2-(piperazin-1-yl)benzonitrile
反応式
[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]参加物
4
反応条件
- 温度
- 122 °C
実験手順
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.
後処理
- temperatureAfter cooling
- customthe mixture is partitioned between dichloromethane
- dry with materialThe organic layers are dried over magnesium sulfate
- concentrationconcentrated
- customThe residue is chromatographed on silica gel
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-9ef007546ddc48d2936bb14ca1172ab3
- 出典データセット
- uspto-grants-2000_01
- 特許番号
- US06013654
反応ノート
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