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Dimethylformamide → HCID 18680816, 화합물

HRID 1699630
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HRID 1699630 반응식
CN(C)C=O.[N+:6]([C:9]1[CH:16]=[CH:15][C:12]([CH2:13]Br)=[CH:11][CH:10]=1)([O-:8])=[O:7].C(=O)(O)[O-].[Na+].[CH3:22][C:23]1[NH:24][C:25]2[CH:31]=[C:30]([C:32](=[O:41])[NH:33][CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][N:36]=3)[CH:29]=[CH:28][C:26]=2[N:27]=1>O.C(Cl)(Cl)Cl>[CH3:22][C:23]1[N:27]([CH2:13][C:12]2[CH:15]=[CH:16][C:9]([N+:6]([O-:8])=[O:7])=[CH:10][CH:11]=2)[C:26]2[CH:28]=[CH:29][C:30]([C:32](=[O:41])[NH:33][CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][N:36]=3)=[CH:31][C:25]=2[N:24]=1
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참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 660114-Nitrobenzyl bromideHCID 516892Sodium BicarbonateHCID 18680895HCID 18680895, 화합물

생성물 1

HCID 18680816HCID 18680816, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 6212
Chloroform
용매

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온도
80 °C

실험 절차

N,N-dimethylformamide (10 ml), 4-nitrobenzyl bromide (3.24 g), and sodium bicarbonate (2.52 g) are added to 2-methyl-5-[(2-pyridylmethyl)carbamoyl]benzimidazole (3.56 g), and the solution is heated for two hours at 80° C. Chloroform and water are added to the reaction solution and layers are separated. After the organic layer is concentrated under reduced pressure, it is purified through silica gel column chromatography (eluate: ethyl acetate/methanol=4/1), and a mixture of 2-methyl-1-(4-nitrobenzyl)-6-[(2-pyridylmethyl)carbamoyl]benzimidazole and 2-methyl-1-(4-nitrobenzyl)-5-[(2-pyridylmethyl)carbamoyl]benzimidazole is obtained. Further, the position isomers in this mixture are separated through medium pressure silica gel column chromatography (eluate: ethyl acetate/methanol=85/15). Each is recrystallized in a mixed solvent of chloroform and diethylether, and thus, 2-methyl-1-(4-nitrobenzyl)-6-[(2-pyridylmethyl)carbamoyl]benzimidazole (1.37 g) (191) and 2-methyl-1-(4-nitrobenzyl)-5-[(2-pyridylmethyl)carbamoyl]benzimidazole (1.19 g) (192) are obtained.

후처리

  1. customare separated
  2. concentrationAfter the organic layer is concentrated under reduced pressure, it
  3. customis purified through silica gel column chromatography (eluate: ethyl acetate/methanol=4/1)
  4. additiona mixture of 2-methyl-1-(4-nitrobenzyl)-6-[(2-pyridylmethyl)carbamoyl]benzimidazole

출처 및 근거

ORD 기록
ord-03a64fcf61844ce2896f1303e9dfb19f
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06348032B1

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