関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Bromo-2,6-difluoroaniline | HCID 610191 | — |
| 生成物 | 5-Bromo-1,3-difluoro-2-nitrobenzene | HCID 21335487 | — |
反応手順
A solution of 4-bromo-2,6-difluoroaniline (240 mmol) in AcOH (150 mL) was added dropwise to a suspension of NaBO3.4 H2O (325 mmol) in AcOH (450 mL) at 70° C. during 30 min. Another 2080 mmol of NaBO3.4 H2O were added over 5 h to the mixture. During this period the mixture was stirred at 70° C. The mixture was poured into water and extracted with Et2O. The organic layer was combined with another Et2O solution obtained from another reaction using the same conditions described above. The mixture was concentrated. A precipitate was formed and separated by filtration. The filtrate was concentrated to afford the desired product after flash column chromatography (SiO2, petroleum ether).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09440929B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-3257fcb39fa44c9aa53c83e4c87efeec |
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| 出典メモ | uspto-grants-2016_09 |
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