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

HRID 1008366노트

반응식

HRID 1008366 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-2450a0f36b3d496194d0326ca6f08f3f
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06797823B1

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