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Pyridine → HCID 86270403, 화합물

HRID 2278984
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HRID 2278984 반응식
[C:1](Cl)(Cl)=[O:2].[O:5]1[CH2:9][CH2:8][C@H:7]([N:10]2[CH2:14][CH2:13][NH:12][C:11]2=[O:15])[CH2:6]1.N1C=CC=CC=1.[CH3:22][N:23]1[CH:27]=[C:26]([C:28]2[CH:33]=[C:32]([O:34][C:35]3[CH:36]=[CH:37][C:38]([NH2:41])=[N:39][CH:40]=3)[CH:31]=[CH:30][N:29]=2)[CH:25]=[N:24]1>C(Cl)Cl.O>[CH3:22][N:23]1[CH:27]=[C:26]([C:28]2[CH:33]=[C:32]([O:34][C:35]3[CH:36]=[CH:37][C:38]([NH:41][C:11]([N:12]4[CH2:13][CH2:14][N:10]([C@H:7]5[CH2:8][CH2:9][O:5][CH2:6]5)[C:1]4=[O:2])=[O:15])=[N:39][CH:40]=3)[CH:31]=[CH:30][N:29]=2)[CH:25]=[N:24]1
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7

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HCID 1049Pyridine2회HCID 6371PhosgeneHCID 593227775-(2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yloxy)pyridin-2-amineHCID 90427717HCID 90427717, 화합물

생성물 1

HCID 86270403HCID 86270403, 화합물수율 45%

시약·촉매·용매 2

HCID 962Water
용매
HCID 6344Dichloromethane용매3회

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온도
0 °C

실험 절차

A 0° C. solution of phosgene (20% in toluene, 0.092 mL, 0.174 mmol) in DCM (2 mL) was treated slowly with a solution of Example B6 (26 mg, 0.166 mmol) and pyridine (0.027 mL, 0.331 mmol) in DCM (2 mL), stirred at 0° C. for 0.5 h, then concentrated to dryness. The residue was dissolved in DCM (2 mL), treated with pyridine (0.0400 mL, 0.495 mmol), cooled to 0° C., treated slowly with a solution of Example A2 (36 mg, 0.165 mmol) in DCM (2 mL), warmed to RT and stirred for 1.5 h. The mixture was diluted with water, extracted with DCM and the organic layer was washed with water, then brine, dried over Na2SO4, concentrated to dryness and purified via silica gel chromatography (MeOH/DCM) to afford (S)—N-(5-((2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yl)oxy)pyridin-2-yl)-2-oxo-3-(tetrahydrofuran-3-yl)imidazolidine-1-carboxamide (33 mg, 45%). 1H NMR (400 MHz, DMSO-d6): δ 10.95 (s, 1 H), 8.38 (d, J=5.8 Hz, 1 H), 8.27 (s, 1 H), 8.23 (d, J=2.9 Hz, 1 H), 8.07 (d, J=9.0 Hz, 1 H), 7.97 (s, 1 H), 7.72 (dd, J=9.0, 2.9 Hz, 1 H), 7.25 (s, 1 H), 6.71 (d, J=5.5 Hz, 1 H), 4.57-4.49 (m, 1 H), 3.91-3.86 (m, 1 H), 3.84 (s, 3 H), 3.83-3.76 (m, 3 H), 3.70-3.57 (m, 2 H), 3.51-3.43 (m, 2 H), 2.19-2.09 (m, 1 H), 2.02-1.91 (m, 1 H); MS (ESI) m/z: 450.1 (M+H+).

후처리

  1. concentrationconcentrated to dryness
  2. dissolutionThe residue was dissolved in DCM (2 mL)
  3. temperaturecooled to 0° C.
  4. temperaturewarmed to RT
  5. stirringstirred for 1.5 h
  6. extractionextracted with DCM
  7. washthe organic layer was washed with water
  8. dry with materialbrine, dried over Na2SO4
  9. concentrationconcentrated to dryness
  10. custompurified via silica gel chromatography (MeOH/DCM)

출처 및 근거

ORD 기록
ord-be8f4a1d4af9425a91fd791563235a08
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09133183B2

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