関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 2-Cyano-4'-methylbiphenyl | HCID 145512 | — |
| 反応物 | Sodium Bromate | HCID 23668195 | — |
| 触媒 | 2,2'-Azobis(2-methylbutyronitrile) | HCID 93079 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | 4'-(Bromomethyl)-2-cyanobiphenyl | HCID 1501912 | 493.9% |
反応手順
4′-Methyl-2-cyanobiphenyl (105 g, 0.54 mol) and sodium bromate (12.3 g, 0.082 mol) were added to monochlorobenzene (300 g) and the internal temperature was set for 65° C. 2,2′-Azobis(2-methylbutyronitrile) (2.0 g, 0.010 mol) was added, bromine (45.6 g, 0.29 mol) was added dropwise over 5 hr and the reaction mixture was maintained at this temperature for 1 hr. The resulting inorganic salt was filtered off and the reaction mixture was cooled to 5° C. The precipitated crystals were collected by filtration to give 4′-bromomethyl-2-cyanobiphenyl (110 g, 0.405 mol). The yield was 75%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06861549B2 |
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| 出典データセット | uspto-grants-2005_03 |
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| ORD ID | ord-f014279446cc4d9097cad5e0f5cf5f8f |
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| 出典メモ | uspto-grants-2005_03 |
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