N-bromobutanimide → 4-Bromo-2-(bromomethyl)-1-fluorobenzene

HRID 50744

反応式

HRID 50744 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:9])=[C:6]([CH3:8])[CH:7]=1.C1C(=O)N([Br:17])C(=O)C1>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:9])=[C:6]([CH:7]=1)[CH2:8][Br:17]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 1235275-Bromo-2-fluorotoluene

生成物 1

HCID 135532954-Bromo-2-(bromomethyl)-1-fluorobenzene

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

To a solution of 5-bromo-2-fluorotoluene (15 g, 0.079 mole) in CCl4 (150 mL) was added NBS (14.2 g, 0.080 mole). The resulting reaction solution was heated under reflux with the starting material being completely consumed within 2 hr. CCl4 was removed under reduced pressure and the residue was diluted, dissolved in ether, washed with brine (3×), dried over MgSO4, and concentrated. Chromatography in hexane yielded 5-bromo-2-fluorobenzyl bromide. The product was immediately used for the reaction below.

後処理

  1. customThe resulting reaction solution
  2. temperaturewas heated
  3. temperatureunder reflux with the starting material
  4. custombeing completely consumed within 2 hr
  5. customCCl4 was removed under reduced pressure
  6. additionthe residue was diluted
  7. dissolutiondissolved in ether
  8. washwashed with brine (3×)
  9. dry with materialdried over MgSO4
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-a0a7822fbbeb4afd8b2e3c1c1581a734
出典データセット
uspto-grants-2004_03
特許番号
US06713478B2

関連ノート

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