Thionyl Chloride → 3,5-Dichloro-6-ethylpyrazine-2-carbonitrile
反応式
[Cl:1][C:2]1[C:3]([C:11]([NH2:13])=O)=[N:4][C:5]([CH2:9][CH3:10])=[C:6]([Cl:8])[N:7]=1.S(Cl)(Cl)=O>CN(C=O)C>[Cl:1][C:2]1[C:3]([C:11]#[N:13])=[N:4][C:5]([CH2:9][CH3:10])=[C:6]([Cl:8])[N:7]=1参加物
4
実験手順
To a mixture of 3,5-dichloro-6-ethylpyrazine-2-carboxamide (1.0 g) and DMF (15 mL), thionyl chloride (1 mL) was added at room temperature and stirred for 20 minutes. The reaction liquid was poured into ice-cold water and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride and then dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane) to give 3,5-dichloro-6-ethylpyrazine-2-carbonitrile (608 mg) as a slightly yellow oil.
後処理
- additionwas added at room temperature
- customThe reaction liquid
- additionwas poured into ice-cold water
- extractionextracted with ethyl acetate
- washThe organic layer was washed with saturated aqueous sodium chloride
- dry with materialdried over anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane)
出典と根拠
- ORDレコード
- ord-0c7ad0b29e07437d8b38309a8e37f469
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969336B2
反応ノート
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