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Sodium Hydroxide → 4-({[4-(dipropylamino)butyl]amino}methyl)-N,N-bis(1H-imidazol-2-ylmethyl)benzamide

HRID 68629
ノート
印刷プレビュー

反応式

HRID 68629 の反応式
[CH2:1]([N:4]([CH2:48][CH2:49][CH3:50])[CH2:5][CH2:6][CH2:7][CH2:8][NH:9][CH2:10][C:11]1[CH:47]=[CH:46][C:14]([C:15]([N:17]([CH2:32][C:33]2[N:34](COCC[Si](C)(C)C)[CH:35]=[CH:36][N:37]=2)[CH2:18][C:19]2[N:20](COCC[Si](C)(C)C)[CH:21]=[CH:22][N:23]=2)=[O:16])=[CH:13][CH:12]=1)[CH2:2][CH3:3].[OH-].[Na+]>CO.Cl>[CH2:48]([N:4]([CH2:1][CH2:2][CH3:3])[CH2:5][CH2:6][CH2:7][CH2:8][NH:9][CH2:10][C:11]1[CH:12]=[CH:13][C:14]([C:15]([N:17]([CH2:32][C:33]2[NH:34][CH:35]=[CH:36][N:37]=2)[CH2:18][C:19]2[NH:23][CH:22]=[CH:21][N:20]=2)=[O:16])=[CH:46][CH:47]=1)[CH2:49][CH3:50]
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

5

反応物 2

HCID 14798Sodium HydroxideHCID 67163333HCID 67163333、化合物

生成物 1

HCID 116483934-({[4-(dipropylamino)butyl]amino}methyl)-N,N-bis(1H-imidazol-2-ylmethyl)benzamide

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

反応条件

温度
80 °C

実験手順

To a solution of the compound 9 in methanol (2 mL), concentrated hydrochloric acid (2 mL) was added. The reaction mixture was stirred at 80° C. for 5 hours. The reaction mixture was added by an aqueous 5N sodium hydroxide solution and then extracted with dichloromethane. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and then concentrated. The obtained residue was purified by silica gel column chromatography (dichloromethane:methanol:28% ammonia water=80:10:1→80:20:4) to obtain the title compound (21 mg) having the following physical properties.

後処理

  1. extractionextracted with dichloromethane
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customThe obtained residue was purified by silica gel column chromatography (dichloromethane:methanol:28% ammonia water=80:10:1→80:20:4)

出典と根拠

ORDレコード
ord-9db2b9dda76f4443b2bd526b2843f450
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822459B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート