化工社化工社 化学情報印刷レポート · 研究参考用
Water → 6-Bromo-8-chloro-1-methyl-1,2,3,4-tetrahydroquinolin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | 6-Bromo-8-chloro-3,4-dihydroquinolin-2(1H)-one | HCID 70979772 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Bromo-8-chloro-1-methyl-1,2,3,4-tetrahydroquinolin-2-one | HCID 72208284 | 45% |
反応手順
A solution of 6-bromo-8-chloro-3,4-dihydro-1H-quinolin-2-one (7.0 g, 26.9 mmol) in DMF (100 mL) was treated with potassium tert-butoxide (6.0 g, 53.8 mmol) at 0° C. in portions. The resulting mixture was stirred at 0° C. for 30 min before methyl iodide (5.0 g, 35.0 mmol) was added. After stirring for 12 h, the reaction mixture was treated with water, extracted with EtOAc, washed with water and brine in sequence, and dried over anhy. Na2SO4. After removal of solvents under reduced pressure, the crude product (3.3 g, 45% yield) was obtained as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09353081B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-8408db3b99294e7fa358e9fecac5e46d |
| 出典メモ | uspto-grants-2016_05 |