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Bromine → 2-Bromo-1-(4-methyl-3-nitrophenyl)ethan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 3'-Nitro-4'-methylacetophenone | HCID 79246 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Bromo-1-(4-methyl-3-nitrophenyl)ethan-1-one | HCID 3800422 | 99.9% |
反応手順
A solution of 1-(4-methyl-3-nitro-phenyl)ethanone (Sigma-Aldrich, 25.08 g, 0.14 mol) in CH2Cl2 (269 mL) is cooled to 0° C. To this is added bromine (7.17 mL, 0.14 mol) at 0° C. with stirring. The reaction mixture is allowed to warm slowly to rt over a total of 90 minutes. Ice water (500 mL) is added, organics are collected and aqueous layer is extracted with CH2Cl2 (2×250 mL). The organic layers are combined, washed with water, dried with Na2SO4 and concentrated to give the title compound (36.1 g, 99% yield). LCMS m/z=258.3, 260.2 [M+H]+, tR=2.39 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871767B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-c3f1d1931a8242a583beeaf89dc254d6 |
| 出典メモ | uspto-grants-2014_10 |