Methylamine → 2-Benzoyl-3-methylaminocrotononitrile
반응식
[CH3:1][NH2:2].C([Li])CCC.[C:8](/[C:16](=[C:19](/OC)\[CH3:20])/[C:17]#[N:18])(=[O:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>>[C:8](/[C:16](=[C:19](/[NH:2][CH3:1])\[CH3:20])/[C:17]#[N:18])(=[O:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1참가 물질
4
실험 절차
In the glass liner of a stainless steel bomb cooled to -78° is condensed 10 ml. of methylamine. To this is added 0.5 ml. of 2 M n-butyllithium (in hexane), followed by 5.0 g. of 2-benzoyl-3-methoxycrotononitrile. The bomb is sealed and heated on a steam bath overnight. The bomb is then cooled, opened and the contents evaporated. The residue is dissolved in chloroform, passed through a Magnesol® pad and the filtrate is evaporated. The residue is recrystallized from chloroform-hexane yielding the title compound.
후처리
- customcondensed 10 ml
- additionTo this is added 0.5 ml
- customThe bomb is sealed
- temperatureheated on a steam bath overnight
- temperatureThe bomb is then cooled
- customthe contents evaporated
- dissolutionThe residue is dissolved in chloroform
- customthe filtrate is evaporated
- customThe residue is recrystallized from chloroform-hexane yielding the title compound
출처 및 근거
- ORD 기록
- ord-3bd2e707470a4ddaad46da5093edd8bf
- 출처 데이터셋
- uspto-grants-1981_03
- 특허 번호
- US04259256
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