関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 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 | 4-Amino-3,5-dichlorobenzotrifluoride | HCID 141094 | 72.2% |
反応手順
3,4,5-Trichloro-trifluoromethylbenzene (0.681 g, 2.73 mmol), lithium fluoride (7.1 mg, 0.273 mmol) and N-methylpyrrolidone (1.8 ml) are mixed in an autoclave. The autoclave is cooled to −95° C. and then ammonia (1.3 g, 76.4 mmol) is added. The autoclave is then heated at 250° C. and with stirring for 4 h and is subsequently allowed to return to room temperature. The reaction product is extracted by washing with water and with dichloromethane and then the organic phase is evaporated, after having been dried. 0.453 g (1.97 mmol) of 2,6-dichloro-4-trifluoromethylaniline is obtained with a degree of conversion of the 3,4,5-trichloro-trifluoromethylbenzene of 97%, a ratio equal to 83/17 for the selectivity for 2,6-dlchloro-para-trifluoromethylaniline with respect to 2,6-dichloro-meta-trifluoromethylaniline and an 87% yield of 2,6-dichloro-para-trifluoromethylaniline.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06479703B1 |
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| 出典データセット | uspto-grants-2002_11 |
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| ORD ID | ord-6475831cd98b4b2986b7ef106e72a8e5 |
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| 出典メモ | uspto-grants-2002_11 |
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