Potassium Carbonate → 4-{[6-(Trifluoromethyl)-3-pyridinyl]oxy}benzaldehyde

HRID 474650ノート

反応式

HRID 474650 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[N:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.F[C:13]1[CH:20]=[CH:19][C:16]([CH:17]=[O:18])=[CH:15][CH:14]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[F:11][C:2]([F:1])([F:10])[C:3]1[N:8]=[CH:7][C:6]([O:9][C:13]2[CH:20]=[CH:19][C:16]([CH:17]=[O:18])=[CH:15][CH:14]=2)=[CH:5][CH:4]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 27833885-Hydroxy-2-(trifluoromethyl)pyridine

生成物 1

HCID 866662084-{[6-(Trifluoromethyl)-3-pyridinyl]oxy}benzaldehyde収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
130 °C

実験手順

To a solution of 6-(trifluoromethyl)-3-pyridinol (2 g, 12.26 mmol) and 4-fluorobenzaldehyde (1.315 ml, 12.26 mmol) in DMF (50 mL), was added K2CO3 (2.54 g, 18.39 mmol). The mixture was heated at 130° C. overnight. After cooling, the reaction mixture was diluted in water, extracted with EA. The organic phase was washed with water and brine, dried over Na2SO4, concentrated to afford the title compound (3.28 g, 12.26 mmol, 100% yield) as a brown oil. LCMS: rt=3.16 min, [M+H+]=268

後処理

  1. temperatureAfter cooling
  2. extractionextracted with EA
  3. washThe organic phase was washed with water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-665a75e8e036463ba0b3fa63488edd05
出典データセット
uspto-grants-2014_01
特許番号
US08637536B2

反応ノート

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