Thionyl Chloride → 3,5-Dichloro-6-ethylpyrazine-2-carbonitrile
반응식
[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]=1참가 물질
4
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-0c7ad0b29e07437d8b38309a8e37f469
- 출처 데이터셋
- uspto-grants-2015_03
- 특허 번호
- US08969336B2
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