Sodium Iodide → 1-Bromo-3-ethoxy-4-(2-ethoxyethoxy)benzene

HRID 1978741ノート

反応式

HRID 1978741 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([O:9][CH2:10][CH3:11])[CH:3]=1.Br[CH2:13][CH2:14][O:15][CH2:16][CH3:17].[I-].[Na+].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:13][CH2:14][O:15][CH2:16][CH3:17])=[C:4]([O:9][CH2:10][CH3:11])[CH:3]=1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 611412-Bromoethyl ethyl etherHCID 218775414-Bromo-2-ethoxyphenol

生成物 1

HCID 219958181-Bromo-3-ethoxy-4-(2-ethoxyethoxy)benzene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

A suspension of 4-bromo-2-ethoxyphenol (8 g), bromoethylethyl ether (5 ml), sodium iodide (5.5 g) and potassium carbonate (10.2 g) in DMF (10 ml) was stirred under nitrogen atmosphere at 90° C. overnight. The solvent was evaporated, and to the residue was added water. The mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and dried with anhydrous magnesium sulfate. The solvent was evaporated, and the residue was distilled under reduced pressure to give 1-bromo-3-ethoxy-4-(2-ethoxyethoxy)benzene (8.1 g) as yellow oil.

後処理

  1. customThe solvent was evaporated
  2. additionto the residue was added water
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated brine
  5. dry with materialdried with anhydrous magnesium sulfate
  6. customThe solvent was evaporated
  7. distillationthe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-634e959b69c5429c9d5a0e10160dfb97
出典データセット
uspto-grants-2001_05
特許番号
US06235771B1

反応ノート

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