化工社化工社 化学情報印刷レポート · 研究参考用
2-Methylfuran → (1R*,5S*)-2,3,4,4-tetrachloro-1-methyl-8-oxabicyclo[3.2.1]octa-2,6-diene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methylfuran | HCID 10797 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Pentachlorocyclopropane | HCID 22631 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (1R*,5S*)-2,3,4,4-tetrachloro-1-methyl-8-oxabicyclo[3.2.1]octa-2,6-diene | HCID 67533581 | — |
反応手順
Pentachlorocyclopropane (100 g, 0.467 mol) is added to a suspension of potassium hydroxide (31.4 g, 0.56 mol) in 1,4-dioxane (3600 ml) and the mixture is stirred at room temperature for 30 minutes and then heated to 65° C. for a further 30 minutes. 2-Methylfuran (38.36 g, 0.467 mol) is added to the reaction mixture, the temperature is raised to 85-90° C. and the mixture is stirred for 16 hours. The reaction mixture is cooled to room temperature, filtered through a plug of diatomaceous earth and the filtrate evaporated under reduced pressure to give (1R*,5S*)-2,3,4,4-tetrachloro-1-methyl-8-oxabicyclo[3.2.1]octa-2,6-diene (83 g), used without further purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895761B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-a1988e3aaf994a1d8def6bee243e2423 |
| 出典メモ | uspto-grants-2014_11 |