化工社化工社 化学情報印刷レポート · 研究参考用
Acetone → 6-Bromo-2,2,4-trimethyl-1,2-dihydroquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Catechol | HCID 289 | — |
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | 4-Bromoaniline | HCID 7807 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 生成物 | 6-Bromo-2,2,4-trimethyl-1,2-dihydroquinoline | HCID 10729464 | 27% |
反応手順
4-Bromoaniline (50 g, 0.290 mol), magnesium sulfate (250 g, 2 mol), iodine (2.5 g, 0.01 mol) and catechol (2.24 g, 0.020 mol) were combined in acetone (750 mL) in a sealed-tube reaction flask. The reaction vessel was placed in a pre-equilibrated oil bath set at 125° C. and stirred overnight. The reaction mixture was then cooled to room temperature, filtered over a pad of diatomaceous earth, and concentrated in vacuo. Chromatography on silica gel provided 6-bromo-2,2,4-trimethyl-1,2-dihydroquinoline as tan colored crystals (21 g, 27% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06858627B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-bc6bae7813934b2eac71c44d75ed28f3 |
| 出典メモ | uspto-grants-2005_02 |