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

HRID 1502440
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HRID 1502440 반응식
[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
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참가 물질

5

반응물 4

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

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-91b76e7a30f74286b7c5c8f372241a42
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09206175B2

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