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3-Bromobenzyl bromide → 3-Bromobenzylmethylsulfone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Bromobenzyl bromide | HCID 69979 | — |
| 反応物 | Sodium methanesulfinate | HCID 2733271 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Bromobenzylmethylsulfone | HCID 2761416 | 67% |
反応手順
A solution of 3-bromobenzyl bromide (5.0 g, 20 mmol) in dry dimethylformamide (50 ml) at room temperature under an atmosphere of argon was treated portionwise with sodium methanesulfinate (2.0 g, 20 mmol) with stirring. The mixture was stirred at room temperature for 16 h, and then at 50° C. for 0.5 h. The reaction mix was allowed to cool to room temperature and then partitioned between ethyl acetate and water. The organic layer was separated and dried over sodium sulfate and the solvent removed under reduced pressure to give an oil which was purified by column chromatography on a 50 g isolute silica sep-pak column eluting from 0-100% ethyl acetate in petroleum ether to give the title compound as an off-white solid (3.34 g, 67%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741351B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-46b8d8503a9e4212bad9578f9f61605b |
| 出典メモ | uspto-grants-2010_06 |