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Sodium Bicarbonate → 6-(Oxan-4-yl)pyridin-3-amine

HRID 1748499
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1748499
C[Si]([N-][Si](C)(C)C)(C)C.[Li+].F[B-](F)(F)F.C(P(C(C)(C)C)C(C)(C)C)(C)(C)C.Br[C:30]1[CH:31]=[CH:32][C:33]([CH:36]2[CH2:41][CH2:40][O:39][CH2:38][CH2:37]2)=[N:34][CH:35]=1.[F-].C([N+:47](CCCC)(CCCC)CCCC)CCC.C(=O)(O)[O-].[Na+]>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].O1CCCC1.C1(C)C=CC=CC=1>[O:39]1[CH2:40][CH2:41][CH:36]([C:33]2[N:34]=[CH:35][C:30]([NH2:47])=[CH:31][CH:32]=2)[CH2:37][CH2:38]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 516892Sodium BicarbonateHCID 2724141Tetrabutylammonium FluorideHCID 2733832Lithium hexamethyldisilazaneHCID 225027355-bromo-2-(tetrahydro-2H-pyran-4-yl)pyridineHCID 44558591Tri-t-butylphosphine fluoroborate

Produkt 1

HCID 86692451
6-(Oxan-4-yl)pyridin-3-amine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysatorHCID 1140TolueneLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

After 1.0M toluene-solution (9.8 ml) of lithium bis(trimethylsilyl)amide was added to bis(dibenzylideneacetone)palladium (0) (67 mg) and tri-tert-butylphosphine tetrafluoroborate (118 mg) at 70° C. under an atmosphere of nitrogen, a toluene solution (8.2 ml) of 5-bromo-2-(tetrahydro-2H-pyran-4-yl)pyridine (1.97 g) was added dropwise and stirred at the same temperature for 0.5 hour. Next, the reaction solution was cooled to room temperature, 1.0M tetrahydrofuran-solution (7.0 ml) of tetrabutylammonium fluoride was added and stirred at the same temperature for 1.5 hours. After completion of the reaction, a saturated aqueous solution of sodium bicarbonate was added and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated. The resulting residue was purified with silica gel column chromatography (n-hexane/ethyl acetate) to give the titled compound (1.1 g) as a white solid.

Aufarbeitung

  1. stirringstirred at the same temperature for 1.5 hours
  2. customAfter completion of the reaction
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe resulting residue was purified with silica gel column chromatography (n-hexane/ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-9f7957d5786a4d1384289942c085bd20
Quelldatensatz
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09150555B2

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