Triethylamine → 5-amino-1-(2-methylphenyl)-1H-pyrazole-4-carbonitrile
반응식
Cl.[CH3:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][NH2:10].C(O[CH:14]=[C:15]([C:18]#[N:19])[C:16]#[N:17])C.C(N(CC)CC)C>CO>[NH2:19][C:18]1[N:9]([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[CH3:2])[N:10]=[CH:14][C:15]=1[C:16]#[N:17]참가 물질
5
실험 절차
10.2 g (64.4 mmol) of 2-methylphenylhydrazine hydrochloride are suspended with 7.8 g (64.4 mmol) of ethoxymethylenemalononitrile in 100 ml of methanol, and 26.9 ml (193.3 mmol) of triethylamine are added. The reaction mixture is heated to reflux overnight, during which a clear solution forms. The solution is subsequently distilled off under reduced pressure, and the crude product is purified by column chromatography (silica gel, mobile phase dichloromethane). 10.8 g (85% of theory) of the desired product are obtained.
후처리
- additionare added
- temperatureThe reaction mixture is heated
- temperatureto reflux overnight, during which a clear solution forms
- distillationThe solution is subsequently distilled off under reduced pressure
- customthe crude product is purified by column chromatography (silica gel, mobile phase dichloromethane)
출처 및 근거
- ORD 기록
- ord-226bc985da0e4a47ad02ffa309b3260b
- 출처 데이터셋
- uspto-grants-2009_11
- 특허 번호
- US07615558B2
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