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Cesium fluoride → 6-Methyl-1-(2,2,2-trifluoroethyl)-5-(2,3,5-trifluorophenyl)pyridin-2(1H)-one

HRID 588736
ノート
印刷プレビュー

反応式

HRID 588736 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5](=[O:14])[N:6]([CH2:9][C:10]([F:13])([F:12])[F:11])[C:7]=1[CH3:8].[F:15][C:16]1[C:21]([F:22])=[CH:20][C:19]([F:23])=[CH:18][C:17]=1B(O)O.[F-].[Cs+]>C1COCC1.CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C>[CH3:8][C:7]1[N:6]([CH2:9][C:10]([F:13])([F:12])[F:11])[C:5](=[O:14])[CH:4]=[CH:3][C:2]=1[C:17]1[CH:18]=[C:19]([F:23])[CH:20]=[C:21]([F:22])[C:16]=1[F:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 25953Cesium fluorideHCID 40788432,3,5-Trifluorophenylboronic AcidHCID 687511515-Bromo-6-methyl-1-(2,2,2-trifluoroethyl)pyridin-2(1H)-one

生成物 1

HCID 866652086-Methyl-1-(2,2,2-trifluoroethyl)-5-(2,3,5-trifluorophenyl)pyridin-2(1H)-one

試薬・触媒・溶媒 2

HCID 178418851HCID 178418851、化合物触媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

Argon was bubbled through a stirred solution of 5-bromo-6-methyl-1-(2,2,2-trifluoroethyl)pyridin-2(1H)-one (9.43 g, 34.9 mmol) in THF (280 mL) for 15 min. To this solution were added 2,3,5-trifluorophenylboronic acid (12.3 g, 69.8 mmol), then cesium fluoride (10.6 g, 69.8 mmol), and finally bis(tri-tert-butylphosphine)palladium(0) (892 mg, 1.75 mmol), and argon was bubbled through the mixture for 5 min after each addition. The reaction mixture was stirred at ambient temperature for 90 min and was then partitioned between saturated aqueous sodium bicarbonate (500 mL) and EtOAc (600 mL). The organic layer was removed and the aqueous phase was extracted further with EtOAc (300 mL). The combined organic extracts were washed with brine, then dried over sodium sulfate, filtered, and concentrated to dryness in vacuo. The crude product was purified by silica gel chromatography, eluting with a gradient of hexanes:EtOAc—100:0 to 0:100, to give the title compound. MS: m/z=322.0 (M+1).

後処理

  1. additionafter each addition
  2. customwas then partitioned between saturated aqueous sodium bicarbonate (500 mL) and EtOAc (600 mL)
  3. customThe organic layer was removed
  4. extractionthe aqueous phase was extracted further with EtOAc (300 mL)
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated to dryness in vacuo
  9. customThe crude product was purified by silica gel chromatography
  10. washeluting with a gradient of hexanes

出典と根拠

ORDレコード
ord-ba64ee4b03944ae0a5794ee48661fdc7
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09227972B2

反応ノート

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