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Sodium Thiosulfate → N-(2-(difluoro(5-fluoropyridin-2-yl)methyl)-4-((5-methyl-1H-pyrazol-3-yl)amino)quinazolin-8-yl)formamide

HRID 473205
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HRID 473205 반응식
[F:1][C:2]([F:25])([C:18]1[CH:23]=[CH:22][C:21]([F:24])=[CH:20][N:19]=1)[C:3]1[N:12]=[C:11](SC)[C:10]2[C:5](=[C:6]([NH:15][CH:16]=[O:17])[CH:7]=[CH:8][CH:9]=2)[N:4]=1.ClC1C=CC=C(C(OO)=O)C=1.S([O-])([O-])(=O)=S.[Na+].[Na+].C(=O)(O)[O-].[Na+].[CH3:49][C:50]1[NH:54][N:53]=[C:52]([NH2:55])[CH:51]=1>C(Cl)Cl.C1COCC1>[F:1][C:2]([F:25])([C:18]1[CH:23]=[CH:22][C:21]([F:24])=[CH:20][N:19]=1)[C:3]1[N:12]=[C:11]([NH:55][C:52]2[CH:51]=[C:50]([CH3:49])[NH:54][N:53]=2)[C:10]2[C:5](=[C:6]([NH:15][CH:16]=[O:17])[CH:7]=[CH:8][CH:9]=2)[N:4]=1
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반응물 5

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 516892Sodium BicarbonateHCID 86662704N-(2-(difluoro(5-fluoropyridin-2-yl)methyl)-4-(methylthio)quinazolin-8-yl)formamide

생성물 1

HCID 56848813
N-(2-(difluoro(5-fluoropyridin-2-yl)methyl)-4-((5-methyl-1H-pyrazol-3-yl)amino)quinazolin-8-yl)formamide
수율 35%

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 8028Tetrahydrofuran용매

실험 절차

To N-(2-(difluoro(5-fluoropyridin-2-yl)methyl)-4-(methylthio)quinazolin-8-yl)formamide (168 mg, 0.462 mmol) in DCM (5 mL) at 0° C. was added 3-chloroperbenzoic acid (70%, 171 mg, 0.69 mmol) and the mixture stirred for 40 min. The mixture was diluted with DCM and then aq sodium thiosulfate and saturated aq sodium bicarbonate were added. The organic layer was separated, dried over sodium sulfate, and concentrated under reduced pressure. To the residue were added THF (4 mL) and 5-methyl-1H-pyrazol-3-amine (135 mg, 1.38 mmol) and the mixture was stirred at rt for 20 min. The mixture was concentrated under reduced pressure and purified by preparative HPLC (Varian C-18 reverse phase column, eluted with gradient of solvent B=0.05% formic acid/ACN and solvent A=5% ACN/0.05% formic acid/H2O) to afford N-(2-(difluoro(5-fluoropyridin-2-yl)methyl)-4-((5-methyl-1H-pyrazol-3-yl)amino)quinazolin-8-yl)formamide (66 mg, 35%). 1H NMR (300 MHz, DMSO-d6) δ ppm 2.17 (s, 3H) 5.89 (s, 1H) 7.61 (t, J=8.10 Hz, 1H) 7.96-8.11 (m, 2H) 8.37 (d, J=8.29 Hz, 1H) 8.66 (d, J=11.87 Hz, 2H) 8.79 (d, J=7.72 Hz, 1H) 10.24 (s, 1H) 10.77 (br s, 1H) 11.81-12.73 (m, 1H); LC-MS (ESI) m/z 414 (M+H)+.

후처리

  1. customThe organic layer was separated
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. stirringthe mixture was stirred at rt for 20 min
  5. concentrationThe mixture was concentrated under reduced pressure
  6. custompurified by preparative HPLC (Varian C-18 reverse phase column
  7. washeluted with gradient of solvent B=0.05% formic acid/ACN and solvent A=5% ACN/0.05% formic acid/H2O)

출처 및 근거

ORD 기록
ord-42a890da7ac54129afbc5e6367f2f5b7
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08633207B2

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