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Carbon Tetrachloride → 1-(Bromomethyl)-2-chloro-3-methyl-5-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Tetrachloride | HCID 5943 | — |
| 反応物 | Benzoyl Peroxide | HCID 7187 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 2-Chloro-1,3-dimethyl-5-nitrobenzene | HCID 9920569 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(Bromomethyl)-2-chloro-3-methyl-5-nitrobenzene | HCID 18997250 | 70.7% |
反応手順
A mixture of 129 g of 2-chloro-1,3-dimethyl-5-nitrobenzene, 125 g of 1-bromo-2,5-pyrrolidinedione, 12 g of dibenzoyl peroxide and 1200 ml of tetrachloromethane was stirred for 2 hours at reflux temperature using a water separator. Twice there was added an extra portion of 20 g of dibenzoyl peroxide during a refluxing period of 29 hours. After cooling, the reaction mixture was washed with water, dried, filtered and evaporated. The residue was purified by column chromatography (silica gel; CH2Cl2 /hexane 50:50). The eluent of the desired fraction was evaporated, yielding 130 g (70.2%) of 1-(bromomethyl)-2-chloro-3-methyl-5-nitrobenzene (interm. 5).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05480912 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-a2d6793df1834518a51fc3a7edf07cbf |
| 出典メモ | uspto-grants-1996_01 |