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Hydrogen Peroxide → 2-Fluoro-5-iodophenol

HRID 606797
ノート
印刷プレビュー

反応式

HRID 606797 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([I:8])=[CH:4][C:3]=1B(O)O.[OH:12]O.[OH-].[Na+]>O1CCCC1.[O-2].[O-2].[Mn+4]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([I:8])=[CH:4][C:3]=1[OH:12]
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 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 162174502-Fluoro-5-iodophenylboronic acid

生成物 1

HCID 469118322-Fluoro-5-iodophenol

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a cooled solution of 2-fluoro-5-iodophenylboronic acid in tetrahydrofuran (200 mL) at 0° C. add an aqueous solution of 30% hydrogen peroxide (9.92 mL, 103 mmol) dropwise, stir 10 min, and add an aqueous 4 N solution of sodium hydroxide (1.78 mL, 7.12 mmol). Warm the reaction to room temperature and stir overnight. Add manganese dioxide (250 mg) to the reaction, stir 90 min and filter through fluted filter paper. Concentrate and partition the residue between diethyl ether and water. Separate the layers and sequentially wash the organic layer with water and an aqueous saturated solution of sodium chloride. Dry (sodium sulfate), filter and concentrate. Purify the resulting tan oil by silica gel chromatography, eluting with a gradient of 0:100 to 30:70 ethyl acetate:hexanes, to give the title compound as a yellow waxy solid (18.1 g, 65%).

後処理

  1. temperatureWarm
  2. customthe reaction to room temperature
  3. stirringstir overnight
  4. stirringstir 90 min
  5. filtrationfilter
  6. filtrationthrough fluted filter paper
  7. concentrationConcentrate
  8. custompartition the residue between diethyl ether and water
  9. customSeparate the layers
  10. washsequentially wash the organic layer with water
  11. dry with materialDry (sodium sulfate)
  12. filtrationfilter
  13. concentrationconcentrate
  14. customPurify the resulting tan oil by silica gel chromatography
  15. washeluting with a gradient of 0:100 to 30:70 ethyl acetate

出典と根拠

ORDレコード
ord-85b8cbf127b34f26b6a74e6cd07837fc
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915424B2

反応ノート

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