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Sodium periodate → HCID 178432877, 화합물

HRID 1875174
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HRID 1875174 반응식
[Cl:1][C:2]1[N:3]=[C:4]([CH3:30])[NH:5][C:6]=1[C:7]([NH:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([O:18][C:19]2[CH:24]=[C:23]([CH:25]=C)[CH:22]=[C:21]([C:27]#[N:28])[CH:20]=2)[C:12]=1[F:29])=[O:8].I([O-])(=O)(=O)=[O:32].[Na+]>C1COCC1.O.CCOC(C)=O.[Os](=O)(=O)(=O)=O>[Cl:1][C:2]1[N:3]=[C:4]([CH3:30])[NH:5][C:6]=1[C:7]([NH:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([O:18][C:19]2[CH:24]=[C:23]([CH:25]=[O:32])[CH:22]=[C:21]([C:27]#[N:28])[CH:20]=2)[C:12]=1[F:29])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 23667635Sodium periodateHCID 178436594HCID 178436594, 화합물

생성물 1

HCID 178432877HCID 178432877, 화합물수율 94%

시약·촉매·용매 4

HCID 30318Osmium Tetroxide촉매HCID 962Water용매HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-chloro-N-({4-chloro-3-[(3-cyano-5-ethenylphenyl)oxy]-2-fluorophenyl}methyl)-2-methyl-1H-imidazole-5-carboxamide (0.260 g, 0.584 mmol) and sodium periodate (0.375 g, 1.752 mmol) in THF (4 ml) and water (2 ml) was added osmium tetroxide (2.5 weight % in t-butanol) (0.147 ml, 0.012 mmol) and the reaction mixture was stirred at rt for 3 hours. The reaction mixture was diluted with EtOAc and washed with water. The solvent was removed and the crude material was purified via silica gel chromatography to give 4-chloro-N-({4-chloro-3-[(3-cyano-5-formylphenyl)oxy]-2-fluorophenyl}methyl)-2-methyl-1H-imidazole-5-carboxamide (0.245 g, 0.548 mmol, 94% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 9.95 (s, 1H), 8.12 (s, 1H), 8.07 (s, 1H), 7.92 (s, 1H), 7.45-7.56 (m, 1H), 7.27-7.44 (m, 1H), 6.91 (d, 1H), 4.52 (d, 2H), 2.23 (s, 3H).

후처리

  1. washwashed with water
  2. customThe solvent was removed
  3. customthe crude material was purified via silica gel chromatography

출처 및 근거

ORD 기록
ord-5bc35ebf5ccc4206820b02c315c3a08f
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08304419B2

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