Acetic Acid → 4'-Fluoro-2-(4-trifluoromethylphenyl)acetophenone

HRID 1975656

反応式

HRID 1975656 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.C(O)(=[O:22])C.S(=O)(=O)(O)O>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:22])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:17])([F:18])[F:19])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 12168182Benzene, 1-[(4-fluorophenyl)ethynyl]-4-(trifluoromethyl)-

生成物 1

HCID 98172164'-Fluoro-2-(4-trifluoromethylphenyl)acetophenone

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
90 °C

実験手順

To 12.2 g (46 mmol) of 4-fluoro-4'-trifluoromethyltolane, 60 ml of water, 60 ml of acetic acid, 40 ml of sulfuric acid and 13.6 g (46 mmol) of mercuric sulfate were added, and the mixture was stirred at 90° C. for 3.5 hours. After completion of the reaction, water was added to the reaction mixture, and the mixture was extracted with diethyl ether. The extract was dried over anhydrous sodium sulfate, and the solvent was distilled off. The residue was purified by silica gel column chromatography (developing solvent: ethyl acetate/n-hexane=1/9) to obtain 5.1 g of 4'-fluoro-2- (4-trifluoromethylphenyl)acetophenone having a melting point of from 87° to 89° C.

後処理

  1. additionwas added to the reaction mixture
  2. extractionthe mixture was extracted with diethyl ether
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off
  5. customThe residue was purified by silica gel column chromatography (developing solvent: ethyl acetate/n-hexane=1/9)

出典と根拠

ORDレコード
ord-09fb09a549d346f4add477d5cea47913
出典データセット
uspto-grants-1994_02
特許番号
US05288727

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