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Potassium Carbonate → 2-Chloro-4-phenylpyridin-3-amine

HRID 887989
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 887989
C(OC(=O)[NH:7][C:8]1[C:9]([Cl:15])=[N:10][CH:11]=[CH:12][C:13]=1I)(C)(C)C.[C:17]1(B(O)O)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>>[Cl:15][C:9]1[C:8]([NH2:7])=[C:13]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:12]=[CH:11][N:10]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 11430Potassium CarbonateHCID 66827Phenylboronic AcidHCID 24229170(2-Chloro-4-iodo-pyridin-3-yl)-carbamic acid tert-butyl ester

Produkt 1

HCID 108220922-Chloro-4-phenylpyridin-3-amine

Versuchsvorschrift

(2-chloro-4-iodo-pyridin-3-yl)-carbamic acid tert-butyl ester a (4.20 g, 11.8 mmol), phenyl boronic acid (1.90 g, 15.6 mmol), potassium carbonate (2.42 g, 17.5 mmol) and tetrakistriphenylphosphine palladium(0) (0.68 g, 0.59 mmol) were weighed into a 20 ml microwave vial. The vial was evacuated, then purged with nitrogen gas 3 times. 16.7 ml dry DMF was added, then 3.3 ml of water, which had been degassed by bubbling nitrogen through it overnight. The vial was then capped and microwaved at 130° C. for 40 minutes. The resulting solution was poured into 250 ml water and extracted with EtOAc (3×50 ml). The combined organics were dried with MgSO4, filtered and concentrated. The resulting oil was adsorbed onto silica gel and purified by flash chromatography (150 g SiO2, 0% to 40% EtOAc in hexanes) to give 2-chloro-3-amino-4-phenyl pyridine b (0.84 g, 4.1 mmol, 35%) and the Boc-protected 2-chloro-3-amino-4-phenyl pyridine c (1.74 g, 5.7 mmol, 48%) as yellow and white solids, respectively.

Aufarbeitung

  1. customThe vial was evacuated
  2. custompurged with nitrogen gas 3 times
  3. addition16.7 ml dry DMF was added
  4. custom3.3 ml of water, which had been degassed
  5. customby bubbling nitrogen through it overnight
  6. customThe vial was then capped
  7. custommicrowaved at 130° C. for 40 minutes
  8. additionThe resulting solution was poured into 250 ml water
  9. extractionextracted with EtOAc (3×50 ml)
  10. dry with materialThe combined organics were dried with MgSO4
  11. filtrationfiltered
  12. concentrationconcentrated
  13. custompurified by flash chromatography (150 g SiO2, 0% to 40% EtOAc in hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-1280d5806ed8428c963287c0c70ed308
Quelldatensatz
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08247557B2

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