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Potassium Carbonate → HCID 66612439, 화합물

HRID 2174617
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HRID 2174617 반응식
Br[C:2]1[N:6]([CH3:7])[N:5]=[C:4]([CH3:8])[C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=1[Cl:16].C1(P(C2C=CC=CC=2)C2C3OC4C(=CC=CC=4P(C4C=CC=CC=4)C4C=CC=CC=4)C(C)(C)C=3C=CC=2)C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].[F:65][C:66]1[CH:72]=[C:71]([O:73][CH3:74])[CH:70]=[C:69]([F:75])[C:67]=1[NH2:68]>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:16][C:10]1[CH:11]=[C:12]([F:15])[CH:13]=[CH:14][C:9]=1[C:3]1[C:4]([CH3:8])=[N:5][N:6]([CH3:7])[C:2]=1[NH:68][C:67]1[C:69]([F:75])=[CH:70][C:71]([O:73][CH3:74])=[CH:72][C:66]=1[F:65]
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참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 51857632,6-Difluoro-4-methoxyanilineHCID 666126355-bromo-4-(2-chloro-4-fluorophenyl)-1,3-dimethyl-1H-pyrazole2회

생성물 1

HCID 66612439HCID 66612439, 화합물

시약·촉매·용매 2

HCID 167845
palladium(II) acetate
촉매
HCID 312751,4-Dioxane용매

실험 절차

5-Bromo-4-(2-chloro-4-fluorophenyl)-1,3-dimethyl-1H-pyrazole (i.e. the product of Step A) (0.20 g, 0.66 mmol), palladium(II) acetate (15 mg, 0.066 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (76 mg, 0.13 mmol) and powdered potassium carbonate (1.8 g, 13 mmol) were combined in anhydrous 1,4-dioxane (3 mL), and the mixture was sparged with a subsurface stream of N2 gas for 10 min. 2,6-Difluoro-4-methoxyaniline (0.22 g, 1.3 mmol) was added in one portion, and the reaction mixture was heated at reflux for 22 h. The reaction mixture was filtered through Celite® diatomaceous filter aid, and the filter pad was washed with ethyl acetate (20 mL). The filtrate was washed with water (10 mL) and brine (10 mL), dried over MgSO4, and concentrated to leave a semisolid residue. This residue was purified by column chromatography through 5 g of silica gel eluted with a gradient of hexanes/ethyl acetate (20:1 to 1:3) to give the title compound, a compound of the present invention, as a light-brown solid (48 mg).

후처리

  1. customthe mixture was sparged with a subsurface stream of N2 gas for 10 min
  2. temperaturethe reaction mixture was heated
  3. temperatureat reflux for 22 h
  4. filtrationThe reaction mixture was filtered through Celite® diatomaceous filter aid
  5. washthe filter pad was washed with ethyl acetate (20 mL)
  6. washThe filtrate was washed with water (10 mL) and brine (10 mL)
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated
  9. customto leave a semisolid residue
  10. customThis residue was purified by column chromatography through 5 g of silica gel
  11. washeluted with a gradient of hexanes/ethyl acetate (20:1 to 1:3)

출처 및 근거

ORD 기록
ord-7bcf5e9fdd9d4d95b3cd08ec032d10a9
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09062005B2

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