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Nitric Acid → 1-Bromo-4-fluoro-2-methyl-5-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 2-Bromo-5-fluorotoluene | HCID 96743 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 1-Bromo-4-fluoro-2-methyl-5-nitrobenzene | HCID 10036983 | 104.8% |
反応手順
Combine 1-bromo-4-fluoro-2-methylbenzene (30.0 g, 159 mmol) in concentrated sulfuric acid (100 mL), cool to about −5° C., and treat dropwise with nitric acid (11.00 mL, 174 mmol) over 20 minutes. Allow reaction mixture to warm to RT and stir for 30 min. Pour onto crushed ice with stirring and partition with tert-butyl methyl ether (MTBE) (200 mL). Separate the aqueous layer and extract with MTBE (2×50 mL). Combine organic layers, dry and concentrate under reduced pressure to provide 1-bromo-4-fluoro-2-methyl-5-nitrobenzene as an orange-colored viscous oil (39.0 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09334267B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-10aeb7632329498392241d80648555f9 |
| 出典メモ | uspto-grants-2016_05 |