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Hydrochloric Acid → 5-Ethyl-2-methoxy-4'-trifluoromethylbenzophenone

HRID 1391338
ノート
印刷プレビュー

反応式

HRID 1391338 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[F:5][C:6]([F:17])([F:16])[C:7]1[CH:15]=[CH:14][C:10]([C:11](Cl)=[O:12])=[CH:9][CH:8]=1.[CH2:18]([C:20]1[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=1)[CH3:19].Cl>ClCCl>[CH2:18]([C:20]1[CH:21]=[CH:22][C:23]([O:26][CH3:27])=[C:24]([CH:25]=1)[C:11]([C:10]1[CH:14]=[CH:15][C:7]([C:6]([F:17])([F:16])[F:5])=[CH:8][CH:9]=1)=[O:12])[CH3:19]
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 313Hydrochloric AcidHCID 676074-(Trifluoromethyl)benzoyl chlorideHCID 736901-Ethyl-4-methoxybenzeneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 213309645-Ethyl-2-methoxy-4'-trifluoromethylbenzophenone収率 88.5%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

Aluminium chloride (0.6 g, 0.004 mole) was stirred in dichloromethane (2 ml) and treated with 4-trifluoromethylbenzoyl chloride (1 g, 0.0048 mole) (ice-bath cooling) and then with 4-ethylanisole (0.6 g, 0.0044 mole) in dichloromethane (1 ml). The mixture was stirred at room temperature overnight and then poured into ice and concentrated hydrochloric acid and extracted with chloroform. The chloroform solution was washed with 10% NaHCO3 solution (100 ml), dried (MgSO4), filtered and evaporated to leave 5-ethyl-2-methoxy-4'-trifluoromethylbenzophenone (1.2 g) as a yellow oil. The latter was heated in 55% aqueous hydrogen bromide (27.5 ml) at 110°-120° C. for 5 hours. The mixture was evaporated to dryness to leave the required product.

後処理

  1. extractionextracted with chloroform
  2. washThe chloroform solution was washed with 10% NaHCO3 solution (100 ml)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-19b9f76e796a4b278719148d0a15ce32
出典データセット
uspto-grants-1979_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04141995

反応ノート

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