関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 4-Amino-3,5-dichlorobenzotrifluoride | HCID 141094 | — |
| 反応物 | Lithium fluoride | HCID 224478 | — |
| 反応物 | 1,2,3-Trichloro-5-(trifluoromethyl)benzene | HCID 2733399 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 1-Chloro-4-(trifluoromethyl)benzene | HCID 7394 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08507693B2 |
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| 出典データセット | uspto-grants-2013_08 |
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| ORD ID | ord-884e7aea6aaa4078ac2a59a4f2ac92c4 |
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| 出典メモ | uspto-grants-2013_08 |
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