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Ethanedioyl dibromide → 4-Bromo-5,5-dimethylfuran-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanedioyl dibromide | HCID 84841 | — |
| 反応物 | 4-Hydroxy-5,5-dimethyl-2(5H)-furanone | HCID 54720139 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Bromo-5,5-dimethylfuran-2-one | HCID 12671960 | 86.2% |
反応手順
To a solution of 4-hydroxy-5,5-dimethyl-5H-furan-2-one (2.1 g, 16.4 mmol) in DCE (40 mL) and DMF (1.5 mL) at 0° C. was added dropwise oxalyl bromide (3.0 mL, 32 mmol, 2 equiv). The mixture was stirred at room temperature for 4-5 h, and then put in an ice bath. Ice water (100 mL) was added slowly. The mixture was extracted with CH2Cl2 (100 mL). The organic phase was washed with 10% NaHCO3 and again with water, dried over sodium sulfate and evaporated to give the title compound 2.7 g (86% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08877923B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-81dcf85130a4439ebe11d250cf52341f |
| 出典メモ | uspto-grants-2014_11 |