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4-formyl-N,N-bis[(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazol-2-yl)methyl]benzamide → 4-formyl-N,N-bis(1H-imidazol-2-ylmethyl)benzamide

HRID 68649
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인쇄 미리보기

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HRID 68649 반응식
[CH:1]([C:3]1[CH:39]=[CH:38][C:6]([C:7]([N:9]([CH2:24][C:25]2[N:26](COCC[Si](C)(C)C)[CH:27]=[CH:28][N:29]=2)[CH2:10][C:11]2[N:12](COCC[Si](C)(C)C)[CH:13]=[CH:14][N:15]=2)=[O:8])=[CH:5][CH:4]=1)=[O:2]>FC(F)(F)C(O)=O.ClCCl>[CH:1]([C:3]1[CH:4]=[CH:5][C:6]([C:7]([N:9]([CH2:24][C:25]2[NH:26][CH:27]=[CH:28][N:29]=2)[CH2:10][C:11]2[NH:15][CH:14]=[CH:13][N:12]=2)=[O:8])=[CH:38][CH:39]=1)=[O:2]
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참가 물질

3

반응물 1

HCID 866542934-formyl-N,N-bis[(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazol-2-yl)methyl]benzamide

생성물 1

HCID 862254924-formyl-N,N-bis(1H-imidazol-2-ylmethyl)benzamide수율 99.9%

시약·촉매·용매 1

HCID 21863450Trifluoroacetic acid methylene chloride용매

실험 절차

To the compound 40 (1.7 g), a 50% trifluoroacetic acid-dichloromethane solution (10 mL) was added. The reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was concentrated and an aqueous 5N sodium hydroxide solution (15 mL) was added to the residue. The aqueous layer was extracted three times with 50 mL of dichloromethane. The combined organic layer was washed with saturated brine and then dried over anhydrous magnesium sulfate. The solvent was concentrated to obtain the title compound (compound B) (922 mg) having the following physical properties.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additionan aqueous 5N sodium hydroxide solution (15 mL) was added to the residue
  3. extractionThe aqueous layer was extracted three times with 50 mL of dichloromethane
  4. washThe combined organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationThe solvent was concentrated

출처 및 근거

ORD 기록
ord-a30393c4b638466c88b7e494e395eefb
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822459B2

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