참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 2-Chloro-5-nitrobenzotrifluoride | HCID 61213 | — |
| 촉매 | Tetraethylammonium Chloride | HCID 5946 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Phenol, 4-nitro-2-(trifluoromethyl)- | HCID 3014014 | — |
반응 단계
450 g of 2-chloro-5-nitro-benzotrifluoride in 1,250 ml of methanol and 35 g of tetraethylammonium chloride are initially introduced. 1,000 g of an aqueous, 50% strength potassium hydroxide solution are then added dropwise (1 hour), the temperature being kept at a maximum of 40° C. by cooling. About 30 minutes after the addition has ended, the mixture is heated to 80° C. for 6 hours, cooled and rendered acid with concentrated hydrochloric acid. The mixture is extracted several times with 300 ml of methylene chloride each time, and the organic phase is dried with sodium sulphate and freed from the solvent under reduced pressure. About 413 g of crude product, melting point: 90°-95° C., are obtained with a purity of about 95% according to analysis by gas chromatography. After recrystallisation from toluene, or distillation under 0.5 mm, pure 4-nitro-2-trifluoromethylphenol is obtained, melting point: 134° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04225731 |
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| 출처 데이터셋 | uspto-grants-1980_09 |
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| ORD ID | ord-65f8aedb14bb489f9cd955c8f6bc1dcc |
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| 출처 메모 | uspto-grants-1980_09 |
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