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Hydrogen Bromide → 2-Bromo-2,4-dimethylpentan-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | 2,4-Dimethyl-3-pentanone | HCID 11271 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 触媒 | Sodium Carbonate | HCID 10340 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Bromo-2,4-dimethylpentan-3-one | HCID 222575 | 85.7% |
反応手順
2,4-dimethyl-3-pentanone (330 g, 2.89M) in chloroform (800 ml) was cooled in an ice water bath to 10° C. and bromine (462 g, 2.89M) was added slowly over 3 hours. After the addition, a slow stream of nitrogen was introduced to the mixture and HBr gas was slowly evolved from the flask. The nitrogen was left bubbling over a weekend to remove all of the HBr produced and then sodium carbonate (5 g) was added. The reaction mixture was then filtered through Celite and the chloroform removed using a rotary evaporator. Distillation of the crude product using a 1′ (2.54 cm) vigreux gave essentially pure 2-bromo-2,4-dimethyl-3-pentanone (478 g, 2.47M) b.pt. 50-52° C./10 mb (1000 Nm−2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06559118B1 |
| 出典データセット | uspto-grants-2003_05 |
| ORD ID | ord-9814e21addcb449e80b9977d407c4ae5 |
| 出典メモ | uspto-grants-2003_05 |