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Tricyclohexylphosphine → 5-amino-N-(2'-amino-6'-methyl-4,4'-bipyridin-3-yl)-3'-fluoro-2,2'-bipyridine-6-carboxamide

HRID 69974
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HRID 69974 반응식
[NH2:1][C:2]1[C:3]([C:9]([NH:11][C:12]2[CH:13]=[N:14][CH:15]=[CH:16][C:17]=2[C:18]2[CH:23]=[C:22]([CH3:24])[N:21]=[C:20]([N:25](C(OC(C)(C)C)=O)C(OC(C)(C)C)=O)[CH:19]=2)=[O:10])=[N:4][C:5](Br)=[CH:6][CH:7]=1.B1(B2OC(C)(C)C(C)(C)O2)OC(C)(C)C(C)(C)O1.C1(P(C2CCCCC2)C2CCCCC2)CCCCC1.CC([O-])=O.[K+].Br[C:83]1[C:88]([F:89])=[CH:87][CH:86]=[CH:85][N:84]=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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl.CCOC(C)=O.O.O1CCOCC1>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:83]2[C:88]([F:89])=[CH:87][CH:86]=[CH:85][N:84]=2)=[N:4][C:3]=1[C:9]([NH:11][C:12]1[CH:13]=[N:14][CH:15]=[CH:16][C:17]=1[C:18]1[CH:23]=[C:22]([CH3:24])[N:21]=[C:20]([NH2:25])[CH:19]=1)=[O:10]
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참가 물질

11

반응물 5

HCID 75806TricyclohexylphosphineHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 27628032-Bromo-3-fluoropyridineHCID 86669206HCID 86669206, 화합물

생성물 1

HCID 690430875-amino-N-(2'-amino-6'-methyl-4,4'-bipyridin-3-yl)-3'-fluoro-2,2'-bipyridine-6-carboxamide

시약·촉매·용매 5

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 178418807HCID 178418807, 화합물촉매HCID 962Water용매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

반응 조건

온도
90 °C

실험 절차

To a solution of degassed dioxane (0.03M) was added 3-amino-6-bromo-N-(2′-(di-BOC-amino)-6′-methyl-4,4′-bipyridin-3-yl)picolinamide (1.0 equiv.), bis(pinacolato)diboron (2.0 equiv.), Pd2(dba)3 (0.05 equiv.), PCy3 (0.075 equiv.), and KOAc (3.0 equiv.). The solution was heated to 90° C. for 16 hrs until all starting material was consumed. Filtered the reaction and concentrated the filtrate. The crude was dried under vacuo, then dissolved in DME/2M Na2CO3 (3:1, 0.05M), followed by addition of 2-bromo-3-fluoropyridine (2.0 equiv.) and Pd(dppf)Cl2-DCM (0.10 equiv.). The reaction was heated to 100° C. in an oil bath until consumption of the boronic ester. Cooled to room temperature, added H2O and EtOAc, the organic phase was washed with brine, then dried with Na2SO4, and concentrated. The crude material was purified via SiO2 column chromatography eluting with EtOAc and hexanes (1:1) and the pure product was concentrated and stirred in DCM/TFA (25%) until completion of the deprotection. The reaction was concentrated to dryness and purified via reverse phase HPLC to afford 5-amino-N-(2′-amino-6′-methyl-4,4′-bipyridin-3-yl)-3′-fluoro-2,2′-bipyridine-6-carboxamide. LCMS (m/z): 416.2 (MH+); LC Rt=1.77 min.

후처리

  1. customwas consumed
  2. filtrationFiltered
  3. customthe reaction
  4. concentrationconcentrated the filtrate
  5. customThe crude was dried under vacuo
  6. dissolutiondissolved in DME/2M Na2CO3 (3:1, 0.05M)
  7. temperatureCooled to room temperature
  8. washthe organic phase was washed with brine
  9. dry with materialdried with Na2SO4
  10. concentrationconcentrated
  11. customThe crude material was purified via SiO2 column chromatography
  12. washeluting with EtOAc and hexanes (1:1)
  13. concentrationthe pure product was concentrated
  14. concentrationThe reaction was concentrated to dryness
  15. custompurified via reverse phase HPLC

출처 및 근거

ORD 기록
ord-f361584948794b93b6105c5be7688f57
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822497B2

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