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

HRID 1613964

반응식

HRID 1613964 반응식
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].[Na+].[Na+].[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]

참가 물질

7

반응물 3

HCID 69211-Chloro-2-(trifluoromethyl)benzeneHCID 10340Sodium CarbonateHCID 178418416HCID 178418416, 화합물2회

생성물 1

HCID 98992-(Trifluoromethyl)benzoic acid수율 14.8%

시약·촉매·용매 3

HCID 24290Palladium Chloride촉매HCID 3882352Chiraphos촉매HCID 962Water용매

반응 조건

온도
210 °C

실험 절차

In an autoclave made of metal were placed 18 g of ortho-chlorobenzotrifluoride, 3.5 mg of palladium chloride, 170 mg of bisdiphenylphosphinobutane and 23 g of sodium 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 for 5 hours on a salt bath at a bath temperature of 210° 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 with ether. The ether layer was dried and then concentrated to obtain 2.8 g of ortho-trifluoromethylbenzoic acid.

후처리

  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 with ether
  7. dry with materialThe ether layer was dried
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1c4f0af3f1144aa298d604a1e633c720
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194631

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