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

HRID 59933

反応式

HRID 59933 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-77d2bf5a1eea489e882ac6cc015a40cc
出典データセット
uspto-grants-2016_09
特許番号
US09440929B2

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