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p-Toluenesulfonic acid monohydrate → 7-methyl-3-(3-trifluoromethylphenyl)-7,8-dihydro-6H-cinnolin-5-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | 7-Methyl-3-(3-(trifluoromethyl)phenyl)-1,4,6,7,8-pentahydrocinnolin-5-one | HCID 4246732 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 7-methyl-3-(3-trifluoromethylphenyl)-7,8-dihydro-6H-cinnolin-5-one | HCID 10018012 | 66.1% |
反応手順
To a pyridine solution (1 mL) of 7-methyl-3-(3-trifluoromethylphenyl)-4,6,7,8-tetrahydro-1H-cinnolin-5-one (136.2 mg, 0.44 mmol) obtained in Example 65 was added p-toluenesulfonic acid hydrate (84 mg, 0.44 mmol) and stirred at room temperature for 3 days. The reaction liquid was concentrated, followed by purification of residue obtained with silica gel column chromatography (methylene chloride/methanol=30/1) to obtain an objective compound (89.0 mg, 66.1%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07563893B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-3d65f477759b46d29d8c9eeb51f701ee |
| 出典メモ | uspto-grants-2009_07 |