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

HRID 468923
Notes
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Reaction equation

HRID 468923 reaction equation
[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
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 4

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

Product 1

HCID 679747861-(5-Bromo-4-methyl(2-pyridyl))-2,2,2-trifluoroethylamineYield 62.2%

Procedure

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).

Workup

  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

Sources & evidence

ORD record
ord-f1d304648ab544e7a25cc635edaff1e2
Source dataset
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08623889B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes