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Dimethyl Sulfoxide → 4-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylaniline

HRID 1375756
ノート
印刷プレビュー

反応式

HRID 1375756 の反応式
[H-].[Na+].CS(C)=O.Cl.[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[C:11]([CH3:16])[C:10]=1[CH3:17].Cl[C:19]1[C:28]2[C:23](=[CH:24][C:25]([O:31][CH3:32])=[C:26]([O:29][CH3:30])[CH:27]=2)[N:22]=[CH:21][CH:20]=1>O>[CH3:30][O:29][C:26]1[CH:27]=[C:28]2[C:23](=[CH:24][C:25]=1[O:31][CH3:32])[N:22]=[CH:21][CH:20]=[C:19]2[O:15][C:12]1[CH:13]=[CH:14][C:9]([NH2:8])=[C:10]([CH3:17])[C:11]=1[CH3:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 24758Sodium hydrideHCID 4596104-Chloro-6,7-dimethoxyquinolineHCID 226672204-Amino-2,3-xylenol hydrochloride

生成物 1

HCID 218904394-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylaniline収率 65%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
50 °C

実験手順

Sodium hydride (60 wt %, 0.72 g) was added to dimethyl sulfoxide (10 ml). The mixture was stirred at 50° C. for 30 min and was then cooled to room temperature. 4-Amino-2,3-dimethylphenol hydrochloride (1.55 g) was added to the cooled mixture, and the mixture was stirred at room temperature for 10 min. Next, 4-chloro-6,7-dimethoxyquinoline (1.00 g) was added thereto, and the mixture was stirred at 100° C. overnight. Water was added to the reaction solution, followed by extraction with chloroform. The chloroform layer was then washed with a saturated aqueous sodium hydrogencarbonate solution and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and methanol was added to the residue. The precipitated crystal was collected by suction filtration to give 0.94 g (yield 65%) of the title compound.

後処理

  1. temperaturewas then cooled to room temperature
  2. stirringthe mixture was stirred at room temperature for 10 min
  3. stirringthe mixture was stirred at 100° C. overnight
  4. extractionfollowed by extraction with chloroform
  5. washThe chloroform layer was then washed with a saturated aqueous sodium hydrogencarbonate solution
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. customThe solvent was removed by distillation under the reduced pressure, and methanol
  8. additionwas added to the residue
  9. filtrationThe precipitated crystal was collected by suction filtration

出典と根拠

ORDレコード
ord-3ee77c3ad2454349b0aae4e73b63683a
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07169789B2

反応ノート

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