1-Chloro-2-(trifluoromethyl)benzene → 2-(Trifluoromethyl)benzoic acid

HRID 1613963

反応式

HRID 1613963 の反応式
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([F:11])([F:10])[F:9].[C:12](=O)([O-:14])[O-:13].[K+].[K+].[C]=O>[Pd](Cl)Cl.C1(P(C(C(P(C2C=CC=CC=2)C2C=CC=CC=2)C)C)C2C=CC=CC=2)C=CC=CC=1.O>[F:9][C:8]([F:11])([F:10])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[C:12]([OH:14])=[O:13]

参加物

7

反応物 3

HCID 69211-Chloro-2-(trifluoromethyl)benzeneHCID 11430Potassium CarbonateHCID 178418416HCID 178418416、化合物2 回

生成物 1

HCID 98992-(Trifluoromethyl)benzoic acid収率 91.5%

試薬・触媒・溶媒 3

HCID 24290Palladium Chloride触媒HCID 3882352Chiraphos触媒HCID 962Water溶媒

反応条件

温度
240 °C

実験手順

In an autoclave made of metal were placed 18 g of ortho-chlorobenzotrifluoride, 3.5 mg of palladium chloride, 170 mg of bisdiphenylphosphinobutane and 3.1 g of potassium carbonate. The air in the autoclave was replaced with carbon monoxide introduced thereinto in several times, after which carbon monoxide was further introduced to adjust its pressure therein to 30 kg/cm2. The reaction was carried out with stirring on a salt bath at a bath temperature of 240° C. After completion of the reaction, the reaction mixture was cooled to room temperature and water was added. The aqueous layer was separated and then acid was added thereto, followed by extraction from the aqueous layer. The ether layer was dried and then concentrated to obtain 3.9 g of ortho-trifluoromethylbenzoic acid.

後処理

  1. additionintroduced
  2. customAfter completion of the reaction
  3. temperaturethe reaction mixture was cooled to room temperature
  4. customThe aqueous layer was separated
  5. additionacid was added
  6. extractionfollowed by extraction from the aqueous layer
  7. dry with materialThe ether layer was dried
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-a96233ecf6c3490fac4a02b62c4ef30e
出典データセット
uspto-grants-1993_03
特許番号
US05194631

関連ノート

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