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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2,2'-[(benzylimino)bis(methylene)]bis(N,N-dimethyl-1H-imidazole-1-sulfonamide) → 2,2'-[iminobis(methylene)]bis(N,N-dimethyl-1H-imidazole-1-sulfonamide)

HRID 1920127
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HRID 1920127 반응식
C([N:8]([CH2:21][C:22]1[N:23]([S:27]([N:30]([CH3:32])[CH3:31])(=[O:29])=[O:28])[CH:24]=[CH:25][N:26]=1)[CH2:9][C:10]1[N:11]([S:15]([N:18]([CH3:20])[CH3:19])(=[O:17])=[O:16])[CH:12]=[CH:13][N:14]=1)C1C=CC=CC=1>[OH-].[Pd+2].[OH-].[C].C(O)C>[NH:8]([CH2:9][C:10]1[N:11]([S:15]([N:18]([CH3:20])[CH3:19])(=[O:16])=[O:17])[CH:12]=[CH:13][N:14]=1)[CH2:21][C:22]1[N:23]([S:27]([N:30]([CH3:32])[CH3:31])(=[O:29])=[O:28])[CH:24]=[CH:25][N:26]=1
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참가 물질

4

반응물 1

HCID 675008132,2'-[(benzylimino)bis(methylene)]bis(N,N-dimethyl-1H-imidazole-1-sulfonamide)

생성물 1

HCID 672857942,2'-[iminobis(methylene)]bis(N,N-dimethyl-1H-imidazole-1-sulfonamide)수율 62.9%

시약·촉매·용매 2

HCID 178502593HCID 178502593, 화합물촉매HCID 702Ethanol용매

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온도
60 °C

실험 절차

To an ethanol (350 mL) solution of the compound (55.7 g) obtained in Example 2, 20% palladium hydroxide-carbon (13.6 g) was added under an argon atmosphere. The reaction mixture was stirred under a hydrogen atmosphere at 60° C. for 6 hours. The reaction mixture was cooled to room temperature and then filtered through Celite. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate:10%-saturated aqueous ammonia-methanol=1:0→8:2) to obtain the title compound (28.5 g) having the following physical properties.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationfiltered through Celite
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by silica gel chromatography (ethyl acetate:10%-saturated aqueous ammonia-methanol=1:0→8:2)

출처 및 근거

ORD 기록
ord-0db4db9d85894a33a1931cd77632cdb9
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08168783B2

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