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Methylamine → 2-Benzoyl-3-methylaminocrotononitrile

HRID 2051628
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인쇄 미리보기

반응식

HRID 2051628 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]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6329MethylamineHCID 234685002-Benzoyl-3-methoxycrotononitrileHCID 178418339Butyllithium

생성물 1

HCID 234685252-Benzoyl-3-methylaminocrotononitrile

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

  1. customcondensed 10 ml
  2. addition
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
To 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-fe8cbf89a45f49edb4113ca84e483a10
    출처 데이터셋
    uspto-grants-1980_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04181677

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