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Hydrochloric Acid → 3,4-Dibromo-6-ethoxy-2-fluorophenol

HRID 1295942
ノート
印刷プレビュー

反応式

HRID 1295942 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH3:10])[C:5]([O:11]CC)=[C:4]([F:14])[C:3]=1[Br:15].[Cl-].[Al+3].[Cl-].[Cl-].Cl>ClCCl>[Br:15][C:3]1[C:4]([F:14])=[C:5]([OH:11])[C:6]([O:8][CH2:9][CH3:10])=[CH:7][C:2]=1[Br:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6451240Aluminum(III) ChlorideHCID 117098891,2-Dibromo-4,5-diethoxy-3-fluorobenzene

生成物 1

HCID 229297133,4-Dibromo-6-ethoxy-2-fluorophenol収率 94%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

After dissolving 1,2-dibromo-3-fluoro-4,5-diethoxybenzene (5 g, 14.5 ml) in dichloromethane (70 ml), aluminum chloride (3.9 g, 29.3 mmol) was added while stirring on ice. The mixture was stirred at room temperature for 2 hours 30 minutes, 1 N hydrochloric acid (70 ml) was added and extraction was performed with ethyl acetate (70 ml×2) and then after washing the combined organic layers with brine (50 ml) and drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to obtain the title compound (4.31 g, 94%).

後処理

  1. additionwas added
  2. stirringThe mixture was stirred at room temperature for 2 hours 30 minutes
  3. extractionextraction
  4. washafter washing the combined organic layers with brine (50 ml)
  5. dry with materialdrying over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-0be36d6136644554a603f7eb634c225e
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07244730B2

反応ノート

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