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Acetone → 7-(4-Chlorobutoxy)-1,2,3,4-tetrahydroquinolin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromo-4-chlorobutane | HCID 81364 | — |
| 反応物 | 7-Hydroxy-3,4-dihydrocarbostyril | HCID 2785758 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 7-(4-Chlorobutoxy)-1,2,3,4-tetrahydroquinolin-2-one | HCID 10467467 | 78% |
反応手順
1-bromo-4-chloro-butane (3.4 g, 20 mmol), anhydrous potassium carbonate powder (4.14 g, 30 mmol) and 7-hydroxy-3,4-dihydro-2(1H)-quinolinone (1.63 g, 10 mmol) are added to 10 ml of acetone and reflux for 24 hours. The reaction solution is evaporated to dryness and dispersed with 20 ml of dichloromethane and 20 ml of water respectively. The organic layer is extracted with water (20 ml×2) and saturated saline (20 ml) successively, dried over anhydrous magnesium sulfate, and evaporated to dryness, to obtain a light yellow powder. The resulting powder is slurried with n-hexane (20 ml×3), filtered, and dried to obtain 1.98 g of 7-(4-chlorobutoxy)-3,4-dihydro-2(1H)-quinolinone, with a yield of 78%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653069B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-fb3ae03c07f64429af56703797c27a50 |
| 出典メモ | uspto-grants-2014_02 |