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Butylamine → N-butyl 3-[(4-bromo-2-methylphenyl)amino]-3-oxopropanamide

HRID 893199
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반응식

HRID 893199 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:16])[CH2:10][C:11]([O:13]CC)=O)=[C:4]([CH3:17])[CH:3]=1.[CH2:18]([NH2:22])[CH2:19][CH2:20][CH3:21]>O.C(O)C>[CH2:18]([NH:22][C:11](=[O:13])[CH2:10][C:9]([NH:8][C:5]1[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][C:4]=1[CH3:17])=[O:16])[CH2:19][CH2:20][CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8007ButylamineHCID 14150214Ethyl 3-[(4-bromo-2-methylphenyl)amino]-3-oxopropanoate

생성물 1

HCID 19096836N-butyl 3-[(4-bromo-2-methylphenyl)amino]-3-oxopropanamide수율 45%

시약·촉매·용매 2

HCID 962Water촉매HCID 702Ethanol용매

실험 절차

A mixture of 4.90 grams (0.02 mole) of ethyl 3-[(4-bromo-2-methylphenyl)amino]-3-oxopropanoate prepared in Example I (Compound No. 75), 358 grams (4.9 moles) of n-butylamine, 150 milliliters of ethanol and 5 drops of water was stirred at room temperature for about 16 hours. After this period, rotary evaporation gave a crude product as a white solid. The white solid was recrystallized from ethyl acetate-hexane to give 3.08 grams (0.009 mole) of N-butyl 3-[(4-bromo-2-methylphenyl)amino]-3-oxopropanamide having a melting point of 123° C.-125° C.

후처리

  1. waitAfter this period
  2. customrotary evaporation
  3. customgave a crude product as a white solid
  4. customThe white solid was recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-67f4ab6fd3974350a68c417d7b3690d2
출처 데이터셋
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05123951

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