3-Chlorotoluene → 3-Methylbenzoic acid

HRID 1613965

反応式

HRID 1613965 の反応式
Cl[C:2]1[CH:3]=[C:4]([CH3:8])[CH:5]=[CH:6][CH:7]=1.C1(P(C(C)C(P(C2C=CC=CC=2)C2C=CC=CC=2)C)C2C=CC=CC=2)C=CC=CC=1.[C:39](=[O:42])([O-])[O-:40].[K+].[K+].[C]=O>[Pd](Cl)Cl.O>[CH3:8][C:4]1[CH:3]=[C:2]([CH:7]=[CH:6][CH:5]=1)[C:39]([OH:40])=[O:42]

参加物

7

反応物 4

HCID 79313-ChlorotolueneHCID 11430Potassium CarbonateHCID 3882352ChiraphosHCID 178418416HCID 178418416、化合物2 回

生成物 1

HCID 74183-Methylbenzoic acid収率 40.4%

試薬・触媒・溶媒 2

HCID 24290Palladium Chloride触媒HCID 962Water溶媒

反応条件

温度
210 °C

実験手順

In an autoclave made of metal were placed 2.53 g of meta-chlorotoluene, 35.5 mg of palladium chloride, 426 mg of bisdiphenylphosphinobutane and 3.04 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 50 kg/cm2. The reaction was carried out with stirring for 3 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, after which acid was added thereto and the deposited crystals were collected by filtration and dried. Thus, 1.10 g of the desired compound meta-methylbenzoic acid was obtained.

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. additionafter which acid was added
  6. filtrationthe deposited crystals were collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-e7ccfce3583a4ef0b88e074ed87bb250
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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