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Methyl iodide → HCID 59674137, 화합물

HRID 1391533
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HRID 1391533 반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:32]=[CH:31][C:12]3[N:13]([CH3:30])[C:14]([N:16]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[N:15][C:11]=3[CH:10]=2)[CH:5]=[CH:4][N:3]=1.[C:33](=O)([O-])[O-].[Cs+].[Cs+].IC>CN(C=O)C>[Cl:1][C:2]1[N:7]=[C:6]([N:8]([CH3:33])[C:9]2[CH:32]=[CH:31][C:12]3[N:13]([CH3:30])[C:14]([N:16]([C:24]4[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=4)[C:17](=[O:23])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[N:15][C:11]=3[CH:10]=2)[CH:5]=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 59674250Tert-butyl 5-[(2-chloropyrimidin-4-yl)amino]-1-methyl-1H-benzimidazol-2-yl(phenyl)carbamate

생성물 1

HCID 59674137HCID 59674137, 화합물수율 78.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Tert-butyl 5-[(2-chloropyrimidin-4-yl)amino]-1-methyl-1H-benzimidazol-2-yl(phenyl)carbamate (0.97 g, 2.2 mmol) was dissolved in DMF (10 ml) and cesium carbonate (2.15 g, 6.6 mmol) was added. After 15 min, iodomethane (0.20 ml, 3.3 mmol) was added, and the reaction was stirred at rt. After TLC showed the starting material to be consumed, the reaction was diluted with water. The aqueous layer was extracted with EtOAc. The combined organic layers were washed with water, dried over MgSO4 and concentrated to a red foam. The crude material was purified through silica gel to give the title compound as a white solid (0.80 g. 78% over two steps). 1H NMR (300 MHz, d6-DMSO) δ 7.90 (d, J=6.3 Hz, 1H), 7.72 (d, J=8.7 Hz, 1H), 7.60 (d, J=1.8 Hz, 1H), 7.38 (m, 4H), 7.25-7.29 (m, 2H), 6.17 (d, J=5.7 Hz, 1H), 3.78 (s, 3H), 3.41 (s, 3H), 1.41 (s, 9H). MS (ESI) m/z=465 [M+H]+.

후처리

  1. customto be consumed
  2. additionthe reaction was diluted with water
  3. extractionThe aqueous layer was extracted with EtOAc
  4. washThe combined organic layers were washed with water
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated to a red foam
  7. customThe crude material was purified through silica gel

출처 및 근거

ORD 기록
ord-9f66503c4d1543d595d52e5d6b2910bb
출처 데이터셋
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07338959B2

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