関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isoquinoline-1-carboxylic acid | HCID 68092 | — |
| 反応物 | N-Methylhydrazinecarbothioamide | HCID 2723853 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | HCID 178418300 | HCID 178418300 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | HCID 178481697 | HCID 178481697 | 78.6% |
反応手順
Hydroxybenzotriazole (0.078 g), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.11 g) and triethylamine were added successively to a cooled solution (0° C.) of 4-methyl-3-thiosemicarbazide (0.061 g) and 1-isoquinoline carboxylic acid (0.10 g) in dimethylformamide (3 ml). Following addition the cooling bath was removed and the mixture was stirred at room temperature over night and then the reaction mixture was evaporated to dryness. To the residue was added sodium hydroxide solution (0.5 M, 5 ml) and the mixture was stirred at 80° C. for 3 h. The mixture was cooled to room temperature and the pH adjusted to pH 6 using hydrochloric acid solution (2M) and the resulting precipitate was filtered and dried in vacuo to give the title compound (0.11 g, 78%) as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07429579B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-bf1242f4a62f4ab2a9d086f066f1c384 |
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| 出典メモ | uspto-grants-2008_09 |
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