Methanol → N-{4-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylphenyl}-N'-(3-fluoro-2-methoxyphenyl)urea

HRID 1008366ノート

反応式

HRID 1008366 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:22]=[CH:21][C:19]([NH2:20])=[C:18]([CH3:23])[C:17]=1[CH3:24].ClC(Cl)(O[C:29](=O)[O:30][C:31](Cl)(Cl)Cl)Cl.[F:37][C:38]1C=CC=[C:40](OC)[C:39]=1N.C[OH:48].C([N:51]([CH2:54]C)[CH2:52][CH3:53])C>C(Cl)(Cl)Cl.ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:22]=[CH:21][C:19]([NH:20][C:54]([NH:51][C:52]2[CH:53]=[CH:40][CH:39]=[C:38]([F:37])[C:29]=2[O:30][CH3:31])=[O:48])=[C:18]([CH3:23])[C:17]=1[CH3:24]

参加物

8

反応物 5

HCID 887MethanolHCID 8471TriethylamineHCID 94429TriphosgeneHCID 4592532-Fluoro-6-methoxyanilineHCID 218904394-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylaniline

生成物 1

HCID 22667166N-{4-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylphenyl}-N'-(3-fluoro-2-methoxyphenyl)urea収率 13%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

4-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylaniline (120 mg) was dissolved in chloroform (10 ml) and triethylamine (1 ml), and a solution of triphosgene (110 mg) in dichloromethane was then added to the solution. The mixture was stirred at room temperature for 30 min. Next, 3-fluoro-o-anisidine (132 μl) was added to the reaction solution, and the mixture was stirred at room temperature for 2 hr. Methanol was added to the reaction solution, and the solvent was removed by distillation under the reduced pressure. The residue was purified by chromatography on silica gel by development with chloroform/methanol (91/9) to give 23 mg (yield 13%) of the title compound.

後処理

  1. stirringthe mixture was stirred at room temperature for 2 hr
  2. customthe solvent was removed by distillation under the reduced pressure
  3. customThe residue was purified by chromatography on silica gel by development with chloroform/methanol (91/9)

出典と根拠

ORDレコード
ord-2450a0f36b3d496194d0326ca6f08f3f
出典データセット
uspto-grants-2004_09
特許番号
US06797823B1

反応ノート

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