関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Chloro-2-(trifluoromethyl)benzene | HCID 6921 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | HCID 178418416 | HCID 178418416 | — |
| 触媒 | Palladium Chloride | HCID 24290 | — |
| 触媒 | Chiraphos | HCID 3882352 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Trifluoromethyl)benzoic acid | HCID 9899 | 14.8% |
反応手順
In an autoclave made of metal were placed 18 g of ortho-chlorobenzotrifluoride, 3.5 mg of palladium chloride, 170 mg of bisdiphenylphosphinobutane and 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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05194631 |
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| 出典データセット | uspto-grants-1993_03 |
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| ORD ID | ord-1c4f0af3f1144aa298d604a1e633c720 |
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| 出典メモ | uspto-grants-1993_03 |
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