Carbon Dioxide → 5-Trifluoromethoxysalicylic acid

HRID 1031885

反応式

HRID 1031885 の反応式
[F:1][C:2]([F:12])([F:11])[O:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.[C:13](=O)([O-:15])[O-:14].[K+].[K+].C(=O)=O>O>[OH:10][C:7]1[CH:6]=[CH:5][C:4]([O:3][C:2]([F:11])([F:12])[F:1])=[CH:9][C:8]=1[C:13]([OH:15])=[O:14]

参加物

5

反応物 3

HCID 280Carbon DioxideHCID 11430Potassium CarbonateHCID 70015p-(Trifluoromethoxy)phenol

生成物 1

HCID 27751035-Trifluoromethoxysalicylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
200 °C

実験手順

178 g (1 mol) of 4-trifluoromethoxyphenol and 345 g (2.5 mol) of potassium carbonate were initially introduced into an autoclave which was then pressurized to 60 bar with carbon dioxide and heated at 200° C. for 4 hours. After cooling and releasing the pressure, the residue was dissolved in 1.5 l of hot water, the solution was filtered hot, the cooled filtrate was extracted using methylene chloride and the extract was clarified using active carbon. The pH was then adjusted to 1 and the precipitated product was filtered off with suction. 192 g of product having a melting point of 129° C. were obtained, which corresponds to 86% of theory.

後処理

  1. temperatureAfter cooling
  2. filtrationthe solution was filtered hot
  3. extractionthe cooled filtrate was extracted
  4. filtrationthe precipitated product was filtered off with suction
  5. customwere obtained

出典と根拠

ORDレコード
ord-753b479947974eae883af69265b3ba90
出典データセット
uspto-grants-1990_09
特許番号
US04956370

関連ノート

読み込み中…