참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | 4-Amino-3,5-dichlorobenzotrifluoride | HCID 141094 | — |
| 반응물 | Lithium fluoride | HCID 224478 | — |
| 반응물 | 1,2,3-Trichloro-5-(trifluoromethyl)benzene | HCID 2733399 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 1-Chloro-4-(trifluoromethyl)benzene | HCID 7394 | — |
반응 단계
WO00/35851/2000 talks about synthesis of 2,6-Dichloro-4-trifluoromethylaniline starting from 3,4,5-trichloro-benzotrifluoride in the presence of alkaline fluorides like lithium fluoride and ammonia in the presence of N-methylpyrrolidone at 250° C. to give 97% conversion and 87% selectivity. The main drawback of the above process is the synthesis of 3,4,5-trichlorobenzotrifluoride in high yield and purity. Chlorination of p-chlorobenzotrifluoride gives a mixture of 3,4,5-trichlorobenzotrifluoride in 72% GLC conversions, 3,4-dichloro and tetrachlorobenzotrifluoride. The process to get pure 3,4,5-isomer from this mixture by fractionation followed by crystallization is very tedious. Moreover in-spite of using very pure intermediates, substantial amount of an undesired isomer (3-amino-4,5-dichlorobenzotrifluoride) is also obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08507693B2 |
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| 출처 데이터셋 | uspto-grants-2013_08 |
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| ORD ID | ord-884e7aea6aaa4078ac2a59a4f2ac92c4 |
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| 출처 메모 | uspto-grants-2013_08 |
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