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4-Isopropylnitrobenzene → 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 | 4-Isopropylnitrobenzene | HCID 15749 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 触媒 | Iron chloride (FeCl3) | HCID 24380 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Bromo-4-nitro-1-(propan-2-yl)benzene | HCID 21531621 | 101.1% |
反応手順
A solution of p-nitrocumene (X) (50 g, 0.300 mol, GC purity: 99.1%) and iron(III) chloride was heated to 40° C. and bromine (59.92 g, 0.375 mol) was added dropwise over a period of 3 hours. The reaction mixture was poured into 120 ml of water, sodium hydrogensulphite (40% strength in water, 20.81 g, 0.078 mol) was added dropwise and the mixture was extracted with 100 ml of chlorobenzene. After phase separation, the chlorobenzene phase was washed with 100 ml of 5% strength aqueous HCl. Removal of the chlorobenzene under reduced pressure gave 2-bromo-1-isopropyl-4-nitrobenzene (74.05 g, 96.9 GC-% by area, 98% of theory) as a 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-0f8ae6945fcf438e85cf6fc99893b49b |
| 出典メモ | uspto-grants-2016_09 |