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3-Aminobenzylamine → N-(3-Aminobenzyl)-10-[(2,2'-dimethyl-1,1'-biphenyl-4-YL)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-C][1,4]benzodiazepine-3-carboxamide

HRID 639231
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HRID 639231 반응식
ClC(Cl)(Cl)[C:3]([C:5]1[N:14]2[C:8]([CH2:9][N:10]([C:19]([C:21]3[CH:26]=[CH:25][C:24]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=4[CH3:33])=[C:23]([CH3:34])[CH:22]=3)=[O:20])[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13]2)=[CH:7][CH:6]=1)=[O:4].[NH2:37][C:38]1[CH:39]=[C:40]([CH:43]=[CH:44][CH:45]=1)[CH2:41][NH2:42]>CS(C)=O.O>[NH2:37][C:38]1[CH:39]=[C:40]([CH:43]=[CH:44][CH:45]=1)[CH2:41][NH:42][C:3]([C:5]1[N:14]2[C:8]([CH2:9][N:10]([C:19]([C:21]3[CH:26]=[CH:25][C:24]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=4[CH3:33])=[C:23]([CH3:34])[CH:22]=3)=[O:20])[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13]2)=[CH:7][CH:6]=1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 46288313-AminobenzylamineHCID 160384712,2,2-Trichloro-1-{10-[(2,2'-dimethyl-1,1'-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone

생성물 1

HCID 16038824N-(3-Aminobenzyl)-10-[(2,2'-dimethyl-1,1'-biphenyl-4-YL)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-C][1,4]benzodiazepine-3-carboxamide수율 57.2%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매
HCID 962
Water
용매

실험 절차

A solution of 2,2,2-trichloro-1-{10-[(2,2′-dimethyl-1,1′-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone of Example 6 (0.125 g; 0.275 mmol), and 3-aminobenzylamine (0.071 g; 0.577 mmol), in dimethylsulfoxide (5 mL) was stirred at 80° C. for 18 hours. The solution was diluted with water and extracted into dichloromethane. The extracts were dried over anhydrous sodium sulfate and evaporated to yield the title compound as an amorphous white solid (0.085 g; 57%), m.p. 105-115° C. MS [(+)ESI, m/z]: 541.2 [M+H]+

후처리

  1. extractionextracted into dichloromethane
  2. dry with materialThe extracts were dried over anhydrous sodium sulfate
  3. customevaporated

출처 및 근거

ORD 기록
ord-e9fd054180c543be8b896c6841f1f8ca
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691848B2

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