関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Dibromobenzene | HCID 7927 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-(Dimethylamino)-1,2-dihydroisoquinolin-1-one | HCID 57424142 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-(3-Bromo-phenyl)-6-dimethylamino-2H-isoquinolin-1-one | HCID 59216430 | 61.9% |
反応手順
6-Dimethylamino-2H-isoquinolin-1-one (39 mg, 0.21 mmol), cuprous iodide (8.0 mg, 0.041 mmol), and potassium carbonate (29 mg, 0.21 mmol) were deposited in sealed vessel. 3 mL DMSO and 1,3-dibromobenzene (98 mg, 0.42 mmol) were added. Argon was bubbled through the mixture for 2 minutes and the lid was tightly closed. This was heated at 150° C. for 5 hours. The resulting mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, concentrated in vacuo, and purified by flash chromatography (25% ethyl acetate/hexanes) to yield 2-(3-Bromo-phenyl)-6-dimethylamino-2H-isoquinolin-1-one (45 mg, 0.13 mmol). MS (ESI) 345.0 (M+H)−.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08299077B2 |
|---|
| 出典データセット | uspto-grants-2012_10 |
|---|
| ORD ID | ord-bd46e15f052346c892daece9c9f2f2ea |
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| 出典メモ | uspto-grants-2012_10 |
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