2-Ethyl-6-methylphenol → 4-Bromo-2-ethyl-6-methylphenol

HRID 363095

反応式

HRID 363095 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:4]=1[OH:10])[CH3:2].[Br-:11].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC>C(Cl)(Cl)Cl>[Br:11][C:7]1[CH:6]=[C:5]([CH3:9])[C:4]([OH:10])=[C:3]([CH2:1][CH3:2])[CH:8]=1

参加物

4

反応物 2

HCID 5193332-Ethyl-6-methylphenolHCID 23500184Tetra-n-butylammonium tribromide

生成物 1

HCID 220068384-Bromo-2-ethyl-6-methylphenol収率 182.7%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Then, 16 g of 2-ethyl-6-methylphenol was dissolved in 200 ml of chloroform, followed by stirring at 0° C., to which 56.6 g of tetrabutylammonium tribromide was added in small portions. After stirring at room temperature for 1 hour, the solvent was removed by distillation under reduced pressure, and the residue was dissolved in 300 ml of diethyl ether. The solution was successively washed with 10% hydrochloric acid and water, dried with anhydrous magnesium sulfate, and concentrated to obtain a crude product. The crude product was subjected to silica gel chromatography, which afforded 23 g of 4-bromo-2-ethyl-6-methylphenol (92% yield).

後処理

  1. additionwas added in small portions
  2. customthe solvent was removed by distillation under reduced pressure
  3. dissolutionthe residue was dissolved in 300 ml of diethyl ether
  4. washThe solution was successively washed with 10% hydrochloric acid and water
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customto obtain a crude product

出典と根拠

ORDレコード
ord-12b1d64a1dd3461ba4f2a029abab3055
出典データセット
uspto-grants-1999_02
特許番号
US05872137

関連ノート

読み込み中…