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Hydrochloric Acid → 1-(5-Bromo-4-methyl(2-pyridyl))-2,2,2-trifluoroethylamine

HRID 468923
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 468923
[Br:1][C:2]1[C:3]([CH3:23])=[CH:4][C:5]([CH:8]([N:13]=CC2C=CC(OC)=CC=2)[C:9]([F:12])([F:11])[F:10])=[N:6][CH:7]=1.O1CCOCC1.Cl.O>>[Br:1][C:2]1[C:3]([CH3:23])=[CH:4][C:5]([CH:8]([NH2:13])[C:9]([F:10])([F:11])[F:12])=[N:6][CH:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 312751,4-DioxaneHCID 711153411-(5-bromo-4-methylpyridin-2-yl)-2,2,2-trifluoro-N-(4-methoxybenzylidene)ethanamine

Produkt 1

HCID 679747861-(5-Bromo-4-methyl(2-pyridyl))-2,2,2-trifluoroethylamineAusbeute 62,2 %

Versuchsvorschrift

To a solution of 1-(5-bromo-4-methylpyridin-2-yl)-2,2,2-trifluoro-N-(4-methoxybenzylidene)ethanamine (77 mg; 0.1989 mmol) in dioxane (1.0 mL; 12 mmol) was added a 1 mol/L solution of hydrochloric acid in water (1.0 mL; 1.0 mmol). The reaction mixture was stirred at room temperature for 2 hours and then heated at 60° C. for 4 hours. The reaction mixture was partitioned between ethyl acetate and water. The layers were separated, and the aqueous layer adjusted to pH 7 with saturated aqueous sodium bicarbonate. The aqueous layer was extracted twice with dichloromethane. The combined dichloromethane extracts were dried over magnesium sulfate, filtered, and concentrated to yield 33.3 mg (62%) of the title compound, which was carried forward without purification. LCMS (ESI): M+H=269.2; 1H NMR (400 MHz, DMSO) δ 8.67 (s, 1H), 7.59 (s, 1H), 4.54 (dd, J=15.9, 7.9 Hz, 1H), 2.55 (d, J=7.8 Hz, 2H), 2.39 (s, 3H).

Aufarbeitung

  1. temperatureheated at 60° C. for 4 hours
  2. customThe reaction mixture was partitioned between ethyl acetate and water
  3. customThe layers were separated
  4. extractionThe aqueous layer was extracted twice with dichloromethane
  5. dry with materialThe combined dichloromethane extracts were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-f1d304648ab544e7a25cc635edaff1e2
Quelldatensatz
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08623889B2

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