関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Quintozene | HCID 6720 | — |
| 反応物 | Tetrachlorofluoronitrobenzene | HCID 13099723 | — |
| 反応物 | Dichlorotrifluoronitrobenzene | HCID 22987219 | — |
| 反応物 | Trichloro-difluoronitrobenzene | HCID 22987224 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1,2-Dichloro-3-fluoro-4-nitrobenzene | HCID 22987215 | 28% |
反応手順
To a reaction vessel, 0.74 g(2.50 m mol) of pentachloronitrobenzene, 1.77 g (13.00 m mol) of DFI, and 25 ml of acetonitrile were charged and reacted at 84° C. for 2 hours in a nitrogen atmosphere. After finishing the reaction, formation of dichlorotrifluoronitrobenzene (master ion, 245, master ion +2 247, master ion +4 249, base peak 245) was confirmed by GC-MS measurement on the reaction mixture, and the yield was 28.0% by GC analysis. Formation of trichloro-difluoronitrobenzene (master ion 261, master ion +2 263, master ion +4 265, base peak 205) was also confirmed and the yield was 11.3%. Formation of tetrachlorofluoronitrobenzene (master ion 277, master ion+2 279, master ion+4 281, master ion+6 283, base peak 221) was further confirmed and the yield was 9.0%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06632949B2 |
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| 出典データセット | uspto-grants-2003_10 |
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| ORD ID | ord-b1e0f89d96b44a378ff0b1f043d741d7 |
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| 出典メモ | uspto-grants-2003_10 |
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