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Cesium fluoride → 6-Chloro-3'-fluoro-4-(pyridazin-4-yl)biphenyl-3-ol

HRID 1619699
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HRID 1619699 반응식
[F-].[Cs+].[Cl:3][C:4]1[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=2)=[CH:8][C:7]([OH:17])=[C:6](I)[CH:5]=1.C([Sn](CCCC)(CCCC)[C:24]1[CH:29]=[CH:28][N:27]=[N:26][CH:25]=1)CCC>C(#N)C.C(OCC)(=O)C.[Cu](I)I.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:3][C:4]1[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=2)=[CH:8][C:7]([OH:17])=[C:6]([C:24]2[CH:29]=[CH:28][N:27]=[N:26][CH:25]=2)[CH:5]=1
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참가 물질

8

반응물 3

HCID 25953Cesium fluorideHCID 64097334-(Tributylstannyl)pyridazineHCID 580423086-Chloro-3'-fluoro-4-iodobiphenyl-3-ol

생성물 1

HCID 1362008776-Chloro-3'-fluoro-4-(pyridazin-4-yl)biphenyl-3-ol수율 85.4%

시약·촉매·용매 4

HCID 83717Copper iodide촉매
HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 6342Acetonitrile용매
HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

Caesium fluoride (219 mg, 1.44 mmol) was added to a solution of 6-chloro-3′-fluoro-4-iodobiphenyl-3-ol (Preparation 99, 251 mg, 0.72 mmol) and 4-(tributylstannyl)pyridazine (345 mg, 0.93 mmol) in acetonitrile (5 mL). The reaction mixture was degassed and copper iodide (28 mg, 0.15 mmol) and tetrakistriphenylphosphinepalladium (0) (83 mg, 0.07 mmol) were added. The reaction mixture was stirred at 80° C. for 3 hours. The cooled reaction mixture was diluted with ethyl acetate (20 mL) and quenched with a solution of ammonia (10%, 10 mL) and stirred for a further 10 minutes. The organic layer was separated and washed with brine (1×10 mL), dried over MgSO4, filtered and concentrated in vacuo. The residue was purified using silica gel chromatography (Biotage) eluting with heptane:ethyl acetate (93:7 to 0:100) to give the title compound (185 mg, 62%) as a yellow solid.

후처리

  1. customThe reaction mixture was degassed
  2. customThe cooled reaction mixture
  3. customquenched with a solution of ammonia (10%, 10 mL)
  4. stirringstirred for a further 10 minutes
  5. customThe organic layer was separated
  6. washwashed with brine (1×10 mL)
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified
  11. washeluting with heptane:ethyl acetate (93:7 to 0:100)

출처 및 근거

ORD 기록
ord-b9c241deedde462cbf745ecbe0469d05
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772293B2

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