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Potassium Carbonate → 5-bromo-N-{6-[5-({[3-(1-cyano-1-methylethyl)phenyl]carbonyl}amino)-2-methylphenoxy][1,2,4]triazolo[1,5-a]pyridin-2-yl}pyridine-3-carboxamide

HRID 1874611
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HRID 1874611 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:8]([OH:10])=O)[CH:5]=[N:6][CH:7]=1.C(Cl)(=O)C(Cl)=O.[NH2:17][C:18]1[N:48]=[C:21]2[CH:22]=[CH:23][C:24]([O:26][C:27]3[CH:28]=[C:29]([NH:34][C:35](=[O:47])[C:36]4[CH:41]=[CH:40][CH:39]=[C:38]([C:42]([C:45]#[N:46])([CH3:44])[CH3:43])[CH:37]=4)[CH:30]=[CH:31][C:32]=3[CH3:33])=[CH:25][N:20]2[N:19]=1.C(=O)([O-])[O-].[K+].[K+].C(=O)([O-])O.[Na+]>O1CCCC1.N1C=CC=CC=1.CO.O1CCCC1.O.CN(C)C=O>[Br:1][C:2]1[CH:3]=[C:4]([C:8]([NH:17][C:18]2[N:48]=[C:21]3[CH:22]=[CH:23][C:24]([O:26][C:27]4[CH:28]=[C:29]([NH:34][C:35]([C:36]5[CH:41]=[CH:40][CH:39]=[C:38]([C:42]([C:45]#[N:46])([CH3:43])[CH3:44])[CH:37]=5)=[O:47])[CH:30]=[CH:31][C:32]=4[CH3:33])=[CH:25][N:20]3[N:19]=2)=[O:10])[CH:5]=[N:6][CH:7]=1
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참가 물질

11

반응물 5

HCID 11430Potassium CarbonateHCID 65578Oxalyl chlorideHCID 887075-Bromonicotinic acidHCID 516892Sodium BicarbonateHCID 68985382N-{3-[(2-amino[1,2,4]triazolo[1,5-a]pyridin-6-yl)oxy]-4-methylphenyl}-3-(1-cyano-1-methylethyl)benzamide

생성물 1

HCID 57749198
5-bromo-N-{6-[5-({[3-(1-cyano-1-methylethyl)phenyl]carbonyl}amino)-2-methylphenoxy][1,2,4]triazolo[1,5-a]pyridin-2-yl}pyridine-3-carboxamide
수율 86%

시약·촉매·용매 5

HCID 962Water용매HCID 1049Pyridine용매HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

To a solution of 5-bromopyridine-3-carboxylic acid (375 mg, 1.87 mmol) in tetrahydrofuran (6 mL) were added oxalyl chloride (204 μL, 2.34 mmol) and N,N-dimethylformamide (20 μL), and the mixture was stirred at room temperature for 1 hr. The reaction mixture was concentrated under reduced pressure. The obtained residue and N-{3-[(2-amino[1,2,4]triazolo[1,5-a]pyridin-6-yl)oxy]-4-methylphenyl}-3-(1-cyano-1-methylethyl)benzamide (400 mg, 0.937 mmol) were dissolved in pyridine (7 mL), and the mixture was stirred at room temperature for 1 hr. Water (15 mL) was added to the reaction mixture, and the mixture was extracted with ethyl acetate (15 mL, 5 mL). The combined organic layer was washed with saturated aqueous sodium hydrogen carbonate solution (3 mL) and saturated brine (2 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. To the obtained residue in methanol-tetrahydrofuran mixed solution (2:1, 6 mL) was added potassium carbonate (130 mg, 0.937 mmol), and the mixture was stirred at room temperature for 14 hr. A saturated aqueous sodium hydrogen carbonate solution (15 mL) was added to the reaction mixture, and the mixture was extracted with ethyl acetate (15 mL, 5 mL). The combined organic layer was washed with saturated brine (5 mL) and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH silica gel, hexane/ethyl acetate=30/70→0/100), and fractions containing the desired product were concentrated under reduced pressure. Diisopropyl ether was added to the obtained residue. The obtained precipitate was collected by filtration and dried to give the title compound (490 mg, 86%) as a colorless powder.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. stirringthe mixture was stirred at room temperature for 1 hr
  3. extractionthe mixture was extracted with ethyl acetate (15 mL, 5 mL)
  4. washThe combined organic layer was washed with saturated aqueous sodium hydrogen carbonate solution (3 mL) and saturated brine (2 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationThe insoluble material was filtered off
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. stirringthe mixture was stirred at room temperature for 14 hr
  9. extractionthe mixture was extracted with ethyl acetate (15 mL, 5 mL)
  10. washThe combined organic layer was washed with saturated brine (5 mL)
  11. dry with materialdried over anhydrous sodium sulfate
  12. filtrationThe insoluble material was filtered off
  13. concentrationthe filtrate was concentrated under reduced pressure
  14. customThe obtained residue was purified by silica gel column chromatography (NH silica gel, hexane/ethyl acetate=30/70→0/100), and fractions
  15. additioncontaining the desired product
  16. concentrationwere concentrated under reduced pressure
  17. additionDiisopropyl ether was added to the obtained residue
  18. filtrationThe obtained precipitate was collected by filtration
  19. customdried

출처 및 근거

ORD 기록
ord-38d3515e60d6447ba44d0a2202e0455e
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08304557B2

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