関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,3-Dichloro-5-(trifluoromethyl)aniline | HCID 13059276 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,2,3-Trichloro-5-(trifluoromethyl)benzene | HCID 2733399 | 55% |
反応手順
A solution of sodium nitrite (39 g.) in water (85 ml.) is added over 1 hour to a solution of 5-amino-3,4-dichloro-α,α,α-trifluorotoluene (117.5 g., 0.51 mol) in 1700 ml. concentrated hydrochloric acid at -6° C. and the solution stirred for 1 hour then filtered. The filtrate is added to a solution of cuprous chloride (76.5 g.) in concentrated hydrochloric acid (500 ml.) over 5 minutes at 0° to 8° C. and gradually heated to 80° C. over 80 minutes. The reaction mixture is cooled to 35° C. and extracted with hexane (2×300 ml.). The extract is washed with water, 2% sodium hydroxide solution, dried and distilled to give 3,4,5-trichloro-α,α,α-trifluorotoluene (70 g., 55%) b.p. 82°-86° C./10 mm, 95% pure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04613360 |
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| 出典データセット | uspto-grants-1986_09 |
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| ORD ID | ord-9f5e5083f00545fc9101c832d7d6f13b |
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| 出典メモ | uspto-grants-1986_09 |
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