関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Aminophenol | HCID 11568 | — |
| 反応物 | 1-Chloro-4-(4-pyridinylmethyl)phthalazine | HCID 1944609 | — |
| 溶媒 | Acetate | HCID 175 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Potassium Carbonate | HCID 11430 | — |
| 生成物 | 1-(3-Hydroxyanilino)-4-(4-pyridylmethyl)phthalazine | HCID 6419391 | — |
反応手順
A mixture of 0.384 g (1.5 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.491 g (4.5 mmol) 3-aminophenol is heated under nitrogen atmosphere for 1 h at 90° C. and for 3 h at 120° C. The reaction mixture is then taken up in a mixture of 30 ml acetate and 20 ml 20% aqueous potassium carbonate solution while stirring for about 4 h, and the filtration material is digested for 20 min in 20 ml of boiling methanol. After cooling to RT, filtration, washing of the filter residue with methanol, and drying under HV (8 h, 130° C.), title compound is obtained with a water content of 1.94%; m.p. 217-219° C.; ESI-MS: (M+H)+=329.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06710047B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-13dac9bc62b74569911d6cec94e6ece0 |
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| 出典メモ | uspto-grants-2004_03 |
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