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Pyridine → HCID 86268825, 화합물

HRID 2279008
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HRID 2279008 반응식
[C:1](Cl)(Cl)=[O:2].[CH3:5][O:6][CH2:7][C@H:8]([N:10]1[CH2:14][CH2:13][NH:12][C:11]1=[O:15])[CH3:9].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.CCOC(C)=O>[CH3:5][O:6][CH2:7][C@H:8]([N:10]1[CH2:14][CH2:13][N:12]([C:11]([NH:41][C:38]2[CH:37]=[CH:36][C:35]([O:34][C:32]3[CH:31]=[CH:30][N:29]=[C:28]([C:26]4[CH:25]=[N:24][N:23]([CH3:22])[CH:27]=4)[CH:33]=3)=[CH:40][N:39]=2)=[O:15])[C:1]1=[O:2])[CH3:9]
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참가 물질

7

반응물 4

HCID 1049PyridineHCID 6371PhosgeneHCID 593227775-(2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yloxy)pyridin-2-amineHCID 90426016HCID 90426016, 화합물

생성물 1

HCID 86268825HCID 86268825, 화합물수율 17.2%

시약·촉매·용매 2

HCID 6344Dichloromethane
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

Phosgene (15% in toluene, 1.75 mL, 2.449 mmol) was treated with a solution of (R)-1-(1-methoxypropan-2-yl)imidazolidin-2-one (155 mg, 0.980 mmol) and pyridine (116 mg, 1.470 mmol) in DCM (2 mL), stirred at RT for 15 min, then concentrated to dryness. The residue was dissolved in DCM (2 mL), treated with a solution of Example A2 (131 mg, 0.490 mmol) and TEA (248 mg, 2.449 mmol) in DCM (2 mL) and stirred at RT for 4 h. The mixture was treated with EtOAc, washed with satd. NaHCO3, then brine, dried over Na2SO4, concentrated to dryness and purified via silica gel chromatography (MeOH/EtOAc) to afford (R)-3-(1-methoxypropan-2-yl)-N-(5-((2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yl)oxy)pyridin-2-yl)-2-oxoimidazolidine-1-carboxamide (38 mg, 17%). 1H NMR (400 MHz, DMSO-d6): δ 10.98 (s, 1 H), 8.37 (d, J=5.7 Hz, 1 H), 8.25 (s, 1 H), 8.22-8.21 (m, 1 H), 8.06-8.05 (m, 1 H), 7.95 (d, J=0.7 Hz, 1 H), 7.72 (dd, J=9.0, 2.9 Hz, 1 H), 7.22 (d, J=2.4 Hz, 1 H), 6.69 (dd, J=5.7, 2.4 Hz, 1 H), 4.10-4.09 (m, 1 H), 3.84 (s, 3 H), 3.81-3.79 (m, 2 H), 3.40-3.39 (m, 4 H), 3.26 (s, 3 H), 1.09 (d, J=6.9 Hz, 3H); MS (ESI) m/z: 452.2 (M+H+).

후처리

  1. concentrationconcentrated to dryness
  2. dissolutionThe residue was dissolved in DCM (2 mL)
  3. stirringstirred at RT for 4 h
  4. washwashed with satd
  5. dry with materialNaHCO3, then brine, dried over Na2SO4
  6. concentrationconcentrated to dryness
  7. custompurified via silica gel chromatography (MeOH/EtOAc)

출처 및 근거

ORD 기록
ord-99bd65751a10424999512ccce4d4cc51
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09133183B2

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