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4-Toluenesulfonyl chloride → 4-({bis[1-(toluene-4-sulfonyl)-1H-imidazol-2-ylmethyl]-amino}-methyl)-N-(4-dipropylaminomethylphenyl)-benzamide

HRID 1173915
ノート
印刷プレビュー

反応式

HRID 1173915 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:6][N:7]([CH2:14][C:15]1[CH:37]=[CH:36][C:18]([C:19]([NH:21][C:22]2[CH:27]=[CH:26][C:25]([CH2:28][N:29]([CH2:33][CH2:34][CH3:35])[CH2:30][CH2:31][CH3:32])=[CH:24][CH:23]=2)=[O:20])=[CH:17][CH:16]=1)[CH2:8][C:9]1[NH:10][CH:11]=[CH:12][N:13]=1.C(N([CH2:43][CH3:44])CC)C.[C:45]1([CH3:55])[CH:50]=[CH:49][C:48]([S:51](Cl)(=[O:53])=[O:52])=[CH:47][CH:46]=1>C(Cl)(Cl)Cl>[C:43]1([CH3:44])[CH:50]=[CH:49][C:48]([S:51]([N:1]2[CH:5]=[CH:4][N:3]=[C:2]2[CH2:6][N:7]([CH2:14][C:15]2[CH:37]=[CH:36][C:18]([C:19]([NH:21][C:22]3[CH:23]=[CH:24][C:25]([CH2:28][N:29]([CH2:33][CH2:34][CH3:35])[CH2:30][CH2:31][CH3:32])=[CH:26][CH:27]=3)=[O:20])=[CH:17][CH:16]=2)[CH2:8][C:9]2[N:13]([S:51]([C:48]3[CH:49]=[CH:50][C:45]([CH3:55])=[CH:46][CH:47]=3)(=[O:53])=[O:52])[CH:12]=[CH:11][N:10]=2)(=[O:53])=[O:52])=[CH:47][CH:46]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 99834204-{[bis(1H-imidazol-2-ylmethyl)-amino]-methyl}-N-(4-dipropylaminomethylphenyl)-benzamide

生成物 1

HCID 588018944-({bis[1-(toluene-4-sulfonyl)-1H-imidazol-2-ylmethyl]-amino}-methyl)-N-(4-dipropylaminomethylphenyl)-benzamide

試薬・触媒・溶媒 1

HCID 6212Chloroform
溶媒
2 回

実験手順

The compound (50.8 mg) obtained in Example 19-3 was dissolved in anhydrous chloroform (2.0 ml). The solution was added with triethylamine (0.049 ml) and then added with p-toluenesulfonyl chloride (manufactured by Kanto Kagaku) (57.2 mg), followed by stirring at room temperature for 16 hours. After completion of the reaction, chloroform (3.0 ml) was added to the solution, and the whole was washed with water. The organic layer was dried with anhydrous magnesium sulfate. Subsequently, the solvent was distilled off and the residue was then purified through silica gel column chromatography (manufactured by Fuji Silysia Chemical Ltd.) (hexane/ethyl acetate), thereby obtaining the subject compound (15.2 mg) as a white solid.

後処理

  1. additionwas added to the solution
  2. washthe whole was washed with water
  3. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  4. distillationSubsequently, the solvent was distilled off
  5. customthe residue was then purified through silica gel column chromatography (manufactured by Fuji Silysia Chemical Ltd.) (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-2763aeafc4804e6786dc4eb919ece842
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07833991B2

反応ノート

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