3-(Trifluoromethyl)phenol → HCID 14512541、化合物

HRID 258327

反応式

HRID 258327 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[C:5]([OH:9])[CH:6]=[CH:7][CH:8]=1.C(N(CC)CC)C.[F:19][C:20](=[CH2:24])[C:21](Cl)=[O:22]>C(Cl)Cl>[F:19][C:20](=[CH2:24])[C:21]([O:9][C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:10])([F:11])[F:1])[CH:4]=1)=[O:22]

参加物

5

反応物 3

HCID 73763-(Trifluoromethyl)phenolHCID 8471TriethylamineHCID 27833352-Fluoroacryloyl chloride

生成物 1

HCID 14512541HCID 14512541、化合物収率 68.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

27.5 g (0.169 mol) of 3-trifluoromethylphenol were dissolved in 100 ml of anhydrous methylene dichloride, and 17.1 g (0.169 mol) of triethylamine were added in portions to the solution; 20 g (0.184 mol) of α-fluoroacryloyl chloride (obtained in accordance with example 1c) were then added dropwise, at a temperature of 5° C., with stirring and in the course of 20 minutes, and the reaction mixture was stirred for a further 60 minutes at the same temperature. The solid formed was filtered off and washed with 30 ml of methylene dichloride. The mixture of filtrate and wash solution was distilled, after adding 0.01 g of hydroquinone monomethyl ether. 27 g (68% of theory) of 3-trifluoromethylphenyl α-fluoroacrylate were obtained, boiling point 78° to 79° C. (under 4 mbar).

後処理

  1. stirringthe reaction mixture was stirred for a further 60 minutes at the same temperature
  2. customThe solid formed
  3. filtrationwas filtered off
  4. washwashed with 30 ml of methylene dichloride
  5. additionThe mixture of filtrate
  6. washwash solution
  7. distillationwas distilled
  8. additionafter adding 0.01 g of hydroquinone monomethyl ether

出典と根拠

ORDレコード
ord-38e232f4472844959dfb9e3b4691fbbe
出典データセット
uspto-grants-1993_11
特許番号
US05266668

関連ノート

読み込み中…