関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methyl-8-hydroxyquinoline | HCID 13224 | — |
| 触媒 | Adams' catalyst | HCID 345198 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Methyl-1,2,3,4-tetrahydroquinolin-8-ol | HCID 3822735 | — |
反応手順
7.50 g (47.0 mmol) of 8-hydroxy-2-methylquinoline were hydrogenated in an autoclave in the presence of 0.75 g of PtO2 in 60 ml of methanol at 4 bar of H2 and a temperature of 50° C. for 24 h. The reaction solution was filtered, and the filtrate was concentrated to dryness. The residue of 2-methyl-8-hydroxy-1,2,3,4-tetrahydroquinoline obtained was dissolved in 60 ml of ethanol, 3.85 ml of 37% strength formaldehyde solution and 1.1 g of Pd/C (10% strength) were added, and the reaction mixture obtained was hydrogenated in an autoclave at 4 bar of H2 and a temperature of 50° C. again for 24 h. It was filtered, the filtrate was concentrated, and the residue was purified by chromatography on SiO2 (EA/n-heptane 1:4). 1.56 g of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06211196B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-c903ed02a5dc468baf72f8ecc3fdc0d3 |
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| 出典メモ | uspto-grants-2001_04 |
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