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Potassium Carbonate → N-{5-[3-(1-methyl-1H-pyrazol-4-yl)-6-quinoxalinyl]-3-pyridinyl}benzenesulfonamide

HRID 734958
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HRID 734958 반응식
Br[C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[CH:7][C:8]([C:12]3[CH:13]=[N:14][N:15]([CH3:17])[CH:16]=3)=[N:9]2)=[CH:4][CH:3]=1.CC1(C)C(C)(C)OB([C:26]2[CH:27]=[C:28]([NH:32][S:33]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)(=[O:35])=[O:34])[CH:29]=[N:30][CH:31]=2)O1.C(=O)([O-])[O-].[K+].[K+]>C(=O)([O-])[O-].[Na+].[Na+].O1CCOCC1.C(OCC)C>[CH3:17][N:15]1[CH:16]=[C:12]([C:8]2[CH:7]=[N:6][C:5]3[C:10]([N:9]=2)=[CH:11][C:2]([C:26]2[CH:27]=[C:28]([NH:32][S:33]([C:36]4[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=4)(=[O:34])=[O:35])[CH:29]=[N:30][CH:31]=2)=[CH:3][CH:4]=3)[CH:13]=[N:14]1
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참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 52936632N-[5-(tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-3-yl]benzenesulfonamide2회HCID 578432587-bromo-2-(1-methyl-1H-pyrazol-4-yl)quinoxaline

생성물 1

HCID 57843521N-{5-[3-(1-methyl-1H-pyrazol-4-yl)-6-quinoxalinyl]-3-pyridinyl}benzenesulfonamide수율 30.4%

시약·촉매·용매 3

HCID 3283
Diethyl Ether
용매
HCID 10340Sodium Carbonate용매
HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

A mixture of 7-bromo-2-(1-methyl-1H-pyrazol-4-yl)quinoxaline (5.98 mmol), N-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3-pyridinyl]benzenesulfonamide (6.78 mmol), and [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) dichloromethane complex (1:1) (0.18 mmol) in 2M aqueous sodium carbonate (15 mL) and 1,4-dioxane (40 mL) was heated at 100° C. for 22 h. Additional N-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3-pyridinyl]benzenesulfonamide (0.83 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) dichloromethane complex (1:1) (0.09 mmol), and 2M aqueous potassium carbonate (3 mL) were added and the reaction mixture was heated at 100° C. for 22 h for complete consumption of starting material. The reaction mixture was cooled, diluted with diethyl ether (30 mL), and filtered through a pad of Celite while rinsing with (2×30 mL) diethyl ether. The organic layer was poured into a separatory funnel containing water (100 mL) and the layers were separated. The aqueous layer was acidified with 6N aqueous HCl until the pH was approximately 7 and then further extracted with (3×200 mL) ethyl acetate. The combined organic layers were dried over sodium sulfate with decolorizing activated carbon, filtered through a pad of Celite while rinsing with (2×100 mL) ethyl acetate, and concentrated in vacuo. The filtrate was separated and the organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo. Recrystallization of the residue from hot ethyl acetate afforded the title product as an ivory solid (804 mg, 30%). Additional product was obtained from the concentrated mother liquors after purification by silica gel chromatography (70-100% ethyl acetate/hexanes) followed by precipitation from cold ethyl acetate (534 mg, 20%). MS(ES)+ m/e 443 [M+H]+.

후처리

  1. temperaturethe reaction mixture was heated at 100° C. for 22 h for complete consumption of starting material
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered through a pad of Celite
  4. washwhile rinsing with (2×30 mL) diethyl ether
  5. additionThe organic layer was poured into a separatory funnel
  6. additioncontaining water (100 mL)
  7. customthe layers were separated
  8. extractionfurther extracted with (3×200 mL) ethyl acetate
  9. dry with materialThe combined organic layers were dried over sodium sulfate
  10. filtrationfiltered through a pad of Celite
  11. washwhile rinsing with (2×100 mL) ethyl acetate
  12. concentrationconcentrated in vacuo
  13. customThe filtrate was separated
  14. dry with materialthe organic layer was dried over sodium sulfate
  15. filtrationfiltered
  16. concentrationconcentrated in vacuo
  17. customRecrystallization of the residue from hot ethyl acetate

출처 및 근거

ORD 기록
ord-c2cad31f43d349a29f6a04c56c5495bc
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07592342B2

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