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HCID 18680797, 화합물 → HCID 18680884, 화합물

HRID 1699631
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HRID 1699631 반응식
[CH3:1][C:2]1[N:6]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][CH:9]=2)[C:5]2[CH:17]=[C:18]([C:21](=[O:30])[NH:22][CH2:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=3)[CH:19]=[CH:20][C:4]=2[N:3]=1.[CH3:31][C:32]1[N:36]([CH2:37][C:38]2[CH:43]=[CH:42][C:41]([N+:44]([O-])=O)=[CH:40][CH:39]=2)[C:35]2[CH:47]=[CH:48][C:49]([C:51](=[O:60])[NH:52][CH2:53][C:54]3[CH:59]=[CH:58][CH:57]=[CH:56][N:55]=3)=[CH:50][C:34]=2[N:33]=1>[Pd].CO>[NH2:14][C:11]1[CH:10]=[CH:9][C:8]([CH2:7][N:6]2[C:5]3[CH:17]=[C:18]([C:21](=[O:30])[NH:22][CH2:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=4)[CH:19]=[CH:20][C:4]=3[N:3]=[C:2]2[CH3:1])=[CH:13][CH:12]=1.[NH2:44][C:41]1[CH:40]=[CH:39][C:38]([CH2:37][N:36]2[C:35]3[CH:47]=[CH:48][C:49]([C:51](=[O:60])[NH:52][CH2:53][C:54]4[CH:59]=[CH:58][CH:57]=[CH:56][N:55]=4)=[CH:50][C:34]=3[N:33]=[C:32]2[CH3:31])=[CH:43][CH:42]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 18680797HCID 18680797, 화합물HCID 18680816HCID 18680816, 화합물

생성물 2

HCID 18680884HCID 18680884, 화합물HCID 18681104HCID 18681104, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

Methanol (30 ml) and 5% palladium/carbon (0.20 g) are added to a mixture (2.32 g) of 2-methyl-1-(4-nitrobenzyl)-6-[(2-pyridylmethyl)carbamoyl]benzimidazole and 2-methyl-1-(4-nitrobenzyl)-5-[(2-pyridylmethyl)carbamoyl]benzimidazole, and the solution is stirred at room temperature under a nitrogen environment until the raw materials dissolved. Solid materials are separated through filtration. The filtrate is concentrated and a residue is obtained. The residue is purified through medium pressure silica gel column chromatography (eluate: ethyl acetate/methanol=85/15), and 1-(4-aminobenzyl)-2-methyl-6-[(2-pyridylmethyl)carbamoyl]benzimidazole and 1-(4-aminobenzyl)-2-methyl-5-[(2-pyridylmethyl)carbamoyl]benzimidazole are separated. These materials are crystallized in mixed solvents of chloroform and diethylether. The crystals are separated through filtration, dried and thus, 1-(4-aminobenzyl)-2-methyl-6-[(2-pyridylmethyl)carbamoyl]benzimidazole (0.354 g) (197) and 1-(4-aminobenzyl)-2-methyl-5-[(2-pyridylmethyl)carbamoyl]benzimidazole (0.330 g) (198) are obtained. 1H-NMR (CDCl3, δ): 3.00 (3H, s), 4.98 (2H, s), 5.88 (2H, s), 7.55 (2H, d, J=8.6 Hz), 7.69 (2H, d, J=8.6 Hz), 7.90 (1H, d, J=8.6 Hz), 7.96 (1H, dt, J=7.1 and 0.6 Hz), 8.12 (1H, J=8.0 Hz), 8.18 (1H, dd, J=8.5 and 1.4 Hz), 8.55 (1H, dt, J=8.0 and 1.7 Hz), 8.62 (1H, d,J=1.1 Hz), 8.77(1H, dd, J=5.9 and 1.1 Hz).

후처리

  1. dissolutiondissolved
  2. customSolid materials are separated through filtration
  3. concentrationThe filtrate is concentrated
  4. customa residue is obtained
  5. customThe residue is purified through medium pressure silica gel column chromatography (eluate: ethyl acetate/methanol=85/15), and 1-(4-aminobenzyl)-2-methyl-6-[(2-pyridylmethyl)carbamoyl]benzimidazole and 1-(4-aminobenzyl)-2-methyl-5-[(2-pyridylmethyl)carbamoyl]benzimidazole
  6. customare separated
  7. customThese materials are crystallized in mixed solvents of chloroform and diethylether
  8. customThe crystals are separated through filtration
  9. customdried

출처 및 근거

ORD 기록
ord-333b11ea43374cde9b1eb571c4808fcd
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06348032B1

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