ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

4-Bromotoluene → 2-Methyl-6-(4-methylphenyl)pyridine

HRID 22256
ノート
印刷プレビュー

反応式

HRID 22256 の反応式
[Mg].Br[C:3]1[CH:8]=[CH:7][C:6]([CH3:9])=[CH:5][CH:4]=1.[CH3:10]C(C[AlH]CC(C)C)C.Br[C:20]1([CH3:26])[CH:25]=[CH:24][CH:23]=C[NH:21]1>O1CCCC1>[CH3:10][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:23]=[CH:24][CH:25]=[C:20]([CH3:26])[N:21]=2)=[CH:5][CH:4]=1
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 4

HCID 78054-BromotolueneHCID 14487Diisobutylaluminum hydrideHCID 5462224Magnesium2 回HCID 686443322-Bromopicoline

生成物 1

HCID 6030812-Methyl-6-(4-methylphenyl)pyridine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Magnesium (1.6 g) and p-bromotoluene (10.2 g) in 100 ml of tetrahydrofuran were stirred and warmed until the reaction commenced. When the exothermic reaction had finished, the mixture was refluxed for 1 hour. In a separate flask, a solution of palladium(II)bis(triphenylphosphine)dichloride (1.4 g) in 60 ml of tetrahydrofuran was prepared, and 4 ml of DIBAL (1M in toluene) added, followed by 2-bromopicoline (6.9 g). To this mixture, the magnesium reagent prepared above was added dropwise, causing an exothermic reaction. The reaction mixture was stirred overnight at room temperature, and then quenched by addition of ether/water. The mixture was washed with dilute hydrochloric acid, water, and then saturated brine. The organic layer was separated, dried over sodium sulfate, the solvent evaporated under reduced pressure, and the residue chromatographed on silica gel, eluting with 30-50% methylene chloride in heptane, to yield 4.5 g of 2-(4-methylphenyl)-6-methylpyridine, a compound of Formula (31), as an oil.

後処理

  1. temperaturewarmed until the reaction commenced
  2. customWhen the exothermic reaction
  3. temperaturethe mixture was refluxed for 1 hour
  4. additionabove was added dropwise
  5. customan exothermic reaction
  6. customquenched by addition of ether/water
  7. washThe mixture was washed with dilute hydrochloric acid, water
  8. customThe organic layer was separated
  9. dry with materialdried over sodium sulfate
  10. customthe solvent evaporated under reduced pressure
  11. customthe residue chromatographed on silica gel
  12. washeluting with 30-50% methylene chloride in heptane

出典と根拠

ORDレコード
ord-69fa0b5b080547718031b61d69c72bad
出典データセット
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05428037

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート