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6-bromo-2-hydroxy-1H-benzo[de]isoquinoline-1,3(2H)-dione → 2-Hydroxy-6-methylthio-benzo[de]isoquinoline-1,3-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 6-bromo-2-hydroxy-1H-benzo[de]isoquinoline-1,3(2H)-dione | HCID 708429 | — |
| 反応物 | Sodium methanethiolate | HCID 4378561 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Hydroxy-6-methylthio-benzo[de]isoquinoline-1,3-dione | HCID 22623968 | 77.1% |
反応手順
Sodium thiomethoxide (0.9 g, 12.0 mmol) was added to a solution of 6-bromo-2-hydroxy-benzo[de]isoquinoline-1,3-dione (1.2 g, 4.0 mmol, from Example 4) in ethanol (200 mL). The mixture was refluxed for 48 hours and concentrated. The solid residue was dissolved in water and acidified with concentrated HCl to pH 4. The resulting precipitate was filtered, washed with water, and dried to give 0.8 g of the title compound, mp 301-206° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06177423B1 |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-845f56130ab94909b2c759e7ba29dc8b |
| 出典メモ | uspto-grants-2001_01 |