N-[4-(diethoxymethyl)benzyl]-N-[(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazol-2-yl)methyl]-1H-imidazole-2-carboxamide → N-(4-formylbenzyl)-N-(1H-imidazol-2-ylmethyl)-1H-imidazole-2-carboxamide

HRID 68635노트

반응식

HRID 68635 반응식
C([O:3][CH:4](OCC)[C:5]1[CH:33]=[CH:32][C:8]([CH2:9][N:10]([CH2:18][C:19]2[N:20](COCC[Si](C)(C)C)[CH:21]=[CH:22][N:23]=2)[C:11]([C:13]2[NH:14][CH:15]=[CH:16][N:17]=2)=[O:12])=[CH:7][CH:6]=1)C>FC(F)(F)C(O)=O.ClCCl>[CH:4]([C:5]1[CH:6]=[CH:7][C:8]([CH2:9][N:10]([CH2:18][C:19]2[NH:20][CH:21]=[CH:22][N:23]=2)[C:11]([C:13]2[NH:17][CH:16]=[CH:15][N:14]=2)=[O:12])=[CH:32][CH:33]=1)=[O:3]

참가 물질

3

실험 절차

To the compound 17 (970 mg), a 50% trifluoroacetic acid-dichloromethane solution (10 mL) was added under ice cooling. The reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was concentrated and an aqueous 2N sodium hydroxide solution (20 mL) was added to the residue. The aqueous layer was extracted twice with dichloromethane (50 mL). The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and then concentrated to obtain the title compound having the following physical properties. The obtained compound was used in the following reaction without being purified.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additionan aqueous 2N sodium hydroxide solution (20 mL) was added to the residue
  3. extractionThe aqueous layer was extracted twice with dichloromethane (50 mL)
  4. washThe combined organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-46777eff6d484156ae59531c7f0e2f50
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822459B2

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