化工社化工社 化学情報印刷レポート · 研究参考用
Triethylsilane → 6-bromo-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylsilane | HCID 12052 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 6-bromo-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran-4-one | HCID 14755364 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 6-bromo-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran | HCID 15840550 | 150.5% |
反応手順
TO a solution of 6-bromo-2,2-dimethyl-2,3-dihydro-4H-1-benzopyran-4-one (7.57 g) in trifluoroacetic acid (21.4 ml) was added at room temperature triethylsilane (10.4 ml), and the mixture was stirred for 4 days. To the mixture was added triethylsilane (7.1 ml), and the mixture was stirred at 50° C. for 24 hours. To the mixture was added at 0° C. 12N sodium hydroxide solution to make the solution alkaline, and the mixture was extracted with diethylether. The organic layer was washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (hexane) to give colorless oil of 6-bromo-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran (10.77 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06235771B1 |
| 出典データセット | uspto-grants-2001_05 |
| ORD ID | ord-f720480f9e6b4f629a9321a3a5635523 |
| 出典メモ | uspto-grants-2001_05 |