関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 反応物 | 6,7-Dimethoxy-4-hydroxyquinoline | HCID 459611 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | 6,7-Dimethoxyquinoline-4(1H)-thione | HCID 22936809 | 74% |
反応手順
After suspending the 6,7-dimethoxy-1H-quinolin-4-one (10.3 g, 50.0 mmol) described in WO9717329, phosphorus pentasulfide (26.7 g, 60.0 mmol) and sodium bicarbonate (26.7 g, 318 mmol) in diglyme (diethyleneglycol dimethyl ether) (100 ml), the suspension was heated and stirred at 80° C. for 2 hours. The reaction solution was returned to room temperature and poured into ice water (1000 ml), and the precipitated crystals were filtered out, washed with water and blow-dried to obtain the title compound (8.19 g, 37.0 mmol, 74%) as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08372981B2 |
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| 出典データセット | uspto-grants-2013_02 |
|---|
| ORD ID | ord-de954c1791554d049741d22c2fa7a9ff |
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| 出典メモ | uspto-grants-2013_02 |
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