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

HRID 68629
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HRID 68629 반응식
[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]
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참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 67163333HCID 67163333, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

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온도
80 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-9db2b9dda76f4443b2bd526b2843f450
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822459B2

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