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Sulfuric Acid → 2-Bromo-4-nitro-1-(propan-2-yl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 1,3-Dibromo-5,5-dimethylhydantoin | HCID 6479 | — |
| 反応物 | 4-Isopropylnitrobenzene | HCID 15749 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Bromo-4-nitro-1-(propan-2-yl)benzene | HCID 21531621 | 202.1% |
反応手順
1,3-Dibromo-5,5-dimethylhydantoin (86.9 g, 0.298 mol) was added in about 5 g portions to a solution of p-nitrocumene (X) (100 g, 0.581 mol, GC purity 96%) and sulphuric acid (178 g, 1.743 mol, 98% strength) over a period of 5 hours. The mixture was then warmed to room temperature and stirred for another 1 hour. The reaction mixture was poured onto 200 g of ice water and admixed with sodium bisulphite (15.1 g, 0.06 mol) and toluene (300 g). The phases were then separated. The organic phase was washed with 5% strength aqueous sodium hydroxide and the toluene was distilled off under reduced pressure. 2-Bromo-1-isopropyl-4-nitrobenzene (147 g, 93.6 GC-% by area, 97% of theory) was obtained as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440908B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-c27b5ded4b3a41ce9c8285a73529adc1 |
| 出典メモ | uspto-grants-2016_09 |