Triethylamine → 5-Bromo-N,N-bis-(4-methoxy-benzyl)-N'-methyl-2-nitro-benzene-1,3-diamine

HRID 59933

반응식

HRID 59933 반응식
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][NH:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)=[CH:5][CH:4]=1.[Br:20][C:21]1[CH:22]=[C:23](F)[C:24]([N+:29]([O-:31])=[O:30])=[C:25]([CH:28]=1)[NH:26][CH3:27].CCN(CC)CC>CCOC(C)=O>[Br:20][C:21]1[CH:28]=[C:25]([NH:26][CH3:27])[C:24]([N+:29]([O-:31])=[O:30])=[C:23]([N:8]([CH2:7][C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:19][CH:18]=2)[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)[CH:22]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 714952Bis(4-methoxybenzyl)amineHCID 716520385-Bromo-3-fluoro-N-methyl-2-nitroaniline

생성물 1

HCID 1182353765-Bromo-N,N-bis-(4-methoxy-benzyl)-N'-methyl-2-nitro-benzene-1,3-diamine

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

A mixture of bis-(4-methoxy-benzyl)-amine (346 mmol), 5-bromo-3-fluoro-N-methyl-2-nitroaniline (297 mmol) and Et3N (891 mmol) was stirred at 120° C. for 16 h. The mixture was then cooled. The crude was combined with another one obtained following the same procedure described above. The resulting mixture was diluted in EtOAc and washed (2×0.2 M HCl, H2O and sat. NaHCO3). The organic phase was dried (Na2SO4) and concentrated to afford the desired product.

후처리

  1. temperatureThe mixture was then cooled
  2. customobtained
  3. washwashed (2×0.2 M HCl, H2O and sat. NaHCO3)
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-77d2bf5a1eea489e882ac6cc015a40cc
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440929B2

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