Hydrochloric Acid → 4-Fluoro-4'-methoxybenzophenone

HRID 225392

反応式

HRID 225392 の反応式
[C:1]1([O:7][CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[F:9][C:10]1[CH:18]=[CH:17][C:13]([C:14](Cl)=[O:15])=[CH:12][CH:11]=1.[Cl-].[Al+3].[Cl-].[Cl-].Cl>O.ClCCl>[F:9][C:10]1[CH:18]=[CH:17][C:13]([C:14]([C:4]2[CH:5]=[CH:6][C:1]([O:7][CH3:8])=[CH:2][CH:3]=2)=[O:15])=[CH:12][CH:11]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 7519AnisoleHCID 678794-Fluorobenzoyl chlorideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 676644-Fluoro-4'-methoxybenzophenone収率 94.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

Anisole (27.5 grams), 4-fluorobenzoyl chloride (35 grams) and dichloromethane (250 mL) were combined in a reaction flask. Aluminum chloride (30.8 grams) was added to the reaction mixture slowly over 20 minutes. Stirred the reaction mixture at room temperature for two hours and then poured it into a mixture of 70 mL concentrated HCl and 500 mL of water. The layers were phase separated and the aqueous layer was extracted with 2 portions of dichloromethane (300 mL each). The organic portions were combined and washed with saturated aqueous sodium bicarbonate (400 mL). The organic layer was dried over anhydrous sodium sulfate and evaporated to yielding 48.0 grams of 4-fluoro-4′-methoxy-benzophenone as a white solid. This material was not purified further but was used directly in the next step.

後処理

  1. additionpoured it
  2. customseparated
  3. extractionthe aqueous layer was extracted with 2 portions of dichloromethane (300 mL each)
  4. washwashed with saturated aqueous sodium bicarbonate (400 mL)
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. customevaporated

出典と根拠

ORDレコード
ord-beed7d87c1d84a6db2065effe62dfba4
出典データセット
uspto-grants-2009_07
特許番号
US07556751B2

関連ノート

読み込み中…