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Sodium Bicarbonate → HCID 21075865, Verbindung

HRID 1374157
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1374157
FC(F)(F)S(O[C:7]1[CH:8]=[N:9][CH:10]=[C:11]([Cl:13])[CH:12]=1)(=O)=O.B1(B2OC(C)(C)C(C)(C)O2)OC(C)(C)C(C)(C)O1.C([O-])(=O)C.[K+].[F:39][C:40]1[CH:45]=[CH:44][CH:43]=[C:42](I)[C:41]=1[C:47]1[N:48]=[N:49][N:50]([CH3:52])[N:51]=1.C(=O)(O)[O-].[Na+]>CN(C=O)C.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]>[Cl:13][C:11]1[CH:10]=[N:9][CH:8]=[C:7]([C:42]2[CH:43]=[CH:44][CH:45]=[C:40]([F:39])[C:41]=2[C:47]2[N:48]=[N:49][N:50]([CH3:52])[N:51]=2)[CH:12]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 516892Sodium BicarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 151858705-Chloropyridin-3-yl trifluoromethanesulfonateHCID 161029015-(2-Fluoro-6-iodophenyl)-2-methyl-2H-tetrazole

Produkt 1

HCID 21075865
HCID 21075865, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)Katalysator2×HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 5-chloropyridin-3-yl trifluoromethanesulfonate (6.00 g, 22.9 mmol), bis(pinacolato)diboron (6.12 g, 24.1 mmol), potassium acetate (6.75 g, 68.8 mmol), and [1,1′-bis-(diphenylphosphino)ferrocene]palladium(II) dichloride (0.60 g, 0.82 mmol) in 30 mL DMF was heated to 80° C. under N2 for 2 hours. The reaction mixture was cooled to room temperature, and 5-(2-fluoro-6-iodophenyl)-2-methyl-2H-tetrazole (4.88 g, 16.1 mmol), sodium bicarbonate (2M, 34.4 mL, 68.8 mmol), and [1,1′-bis(diphenylphosphino)ferrocene]palladium(II) dichloride (0.60 g, 0.82 mmol) were added. The reaction mixture was heated to 80° C. overnight, then cooled to room temperature and partitioned between ethyl acetate and water. The organic extract was washed with water and brine, dried over Na2SO4, filtered and concentrated under vacuum. The residue was subjected to silica gel chromatography eluted with 0–30% ethyl acetate in hexanes to provide 3-chloro-5-[3-fluoro-2-(2-methyl-2H-tetrazol-5-yl)phenyl]pyridine that gave proton NMR spectra consistent with theory and a mass ion (ES+) of 290.11 for M+H+.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to room temperature
  2. temperatureThe reaction mixture was heated to 80° C. overnight
  3. temperaturecooled to room temperature
  4. custompartitioned between ethyl acetate and water
  5. extractionThe organic extract
  6. washwas washed with water and brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum
  10. washeluted with 0–30% ethyl acetate in hexanes

Quellen und Nachweise

ORD-Eintrag
ord-e81b485628114c8f8dc3941b4f58b8c8
Quelldatensatz
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07163951B2

Notizen zur Reaktion

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