참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrogen Peroxide | HCID 784 | — |
| 반응물 | HCID 18997589 | HCID 18997589 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 생성물 | 2,4-Dichloro-5-fluorobenzoic acid | HCID 688138 | 85.2% |
반응 단계
26.8 g (0.1 mol) of 2,4-dichloro-5-fluorobenzophenone are dissolved in 250 g of 96% sulfuric acid, and 17 g of 30% hydrogen peroxide solution are added at 0° C., with thorough mixing, in such a way that the temperature does not exceed 40° C. When the metered addition is complete, the temperature is allowed to drop to 20° C. and the mixture is stirred for 5 h at this temperature. If the conversion is incomplete, a further 5 g of hydrogen peroxide solution are metered in (T<40° C.) and the mixture is diluted with 1000 g of water after a further 3 h of reaction time and is subsequently stirred for 2 h. The 2,4-dichloro-5-fluorobenzoic acid which has precipitated out is filtered off and purified by recrystallization (water) to give 17.8 g (0.0852 mol, 85%) of 2,4-dichloro-5-fluorobenzoic acid melting at 144°-146° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05481032 |
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| 출처 데이터셋 | uspto-grants-1996_01 |
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| ORD ID | ord-f646ca80c5e9470686d0709ce74955f2 |
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| 출처 메모 | uspto-grants-1996_01 |
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