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

HRID 1502440
ノート
印刷プレビュー

反応式

HRID 1502440 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

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

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-91b76e7a30f74286b7c5c8f372241a42
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09206175B2

反応ノート

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