Triethylamine → N-[2-(Dibutylamino)ethyl]-N'-{4-[(6,7-dimethoxy-4-quinolyl)oxy]-2,3-dimethylphenyl}urea

HRID 721581ノート

反応式

HRID 721581 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].C(N(CC)CC)C.ClC(Cl)(O[C:36](=[O:42])OC(Cl)(Cl)Cl)Cl.[CH2:44]([N:48]([CH2:52][CH2:53][CH2:54][CH3:55])[CH2:49][CH2:50][NH2:51])[CH2:45][CH2:46][CH3:47]>C(Cl)(Cl)Cl.O>[CH2:44]([N:48]([CH2:52][CH2:53][CH2:54][CH3:55])[CH2:49][CH2:50][NH:51][C:36]([NH:20][C:19]1[CH:21]=[CH:22][C:16]([O:15][C:6]2[C:5]3[C:10](=[CH:11][C:12]([O:13][CH3:14])=[C:3]([O:2][CH3:1])[CH:4]=3)[N:9]=[CH:8][CH:7]=2)=[C:17]([CH3:24])[C:18]=1[CH3:23])=[O:42])[CH2:45][CH2:46][CH3:47]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 77062N,N-DibutylethylenediamineHCID 94429TriphosgeneHCID 218904394-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylaniline

生成物 1

HCID 21891148N-[2-(Dibutylamino)ethyl]-N'-{4-[(6,7-dimethoxy-4-quinolyl)oxy]-2,3-dimethylphenyl}urea収率 49.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒2 回

実験手順

4-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,3-dimethylaniline (100 mg) was dissolved in chloroform (10 ml) and triethylamine (1 ml) to prepare a solution. A solution of triphosgene (139 mg) in chloroform was then added to the solution, and the mixture was stirred at room temperature for 10 min. Next, N1,N1-dibutyl-1,2-ethanediamine (81 mg) was added thereto, and the mixture was further stirred at room temperature for one hr. Water was added to stop the reaction, and the reaction solution was then extracted with chloroform, followed by concentration. The residue was purified on a column using chloroform/methanol to give the title compound (80 mg, yield 49%).

後処理

  1. stirringthe mixture was further stirred at room temperature for one hr
  2. customthe reaction
  3. extractionthe reaction solution was then extracted with chloroform
  4. concentrationfollowed by concentration
  5. customThe residue was purified on a column

出典と根拠

ORDレコード
ord-39ca04a6ca8f44a9879c817df1cc3220
出典データセット
uspto-grants-2006_11
特許番号
US07135466B2

反応ノート

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