참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,3-Dimethyl-2-imidazolidinone | HCID 6661 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2,3,4-Trifluorobenzoic acid | HCID 302932 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3,4-Difluoro-2-hydroxybenzoic acid | HCID 2758286 | 95.1% |
반응 단계
1.76 g (0.01 mole) of 2,3,4-trifluorobenzoic acid, 1.62 g (0.04 mole) of powdery 99% sodium hydroxide and 20 ml of 1,3-dimethyl-2-imidazolidinone were fed into a 100-ml four-necked flask provided with a thermometer, a stirrer and a reflux condenser. The mixture was stirred at 150° C. for 2 hours to give rise to a reaction. After the completion of the reaction, part of 1,3-dimethyl-2-imidazolidinone was recovered. The resulting reaction mixture was diluted with 500 ml of water and then subjected to precipitation with a 10% aqueous hydrochloric acid solution. The resulting material was cooled in an ice bath. The resulting crystals were collected by filtration, washed with water, and dried to obtain 1.66 g of 3,4-difluorosalicylic acid. The isolated yield was 95.1% relative to the 2,3,4-trifluorobenzoic acid used.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06166246 |
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| 출처 데이터셋 | uspto-grants-2000_12 |
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| ORD ID | ord-210d2c0213b541a2adb95534b5747799 |
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| 출처 메모 | uspto-grants-2000_12 |
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