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Cyanoacetic acid hydrazide → 3-Oxo-5-phenyl-2,3-dihydro-pyridazine-4-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyanoacetic acid hydrazide | HCID 8820 | — |
| 反応物 | Phenylglyoxal | HCID 14090 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Oxo-5-phenyl-2,3-dihydro-pyridazine-4-carbonitrile | HCID 59735096 | — |
反応手順
Phenyl glyoxal (1.0 g, 7.46 mmol) and cyanoacetohydrazide (740 mg, 7.46 mmol) were heated to reflux in 10 mL ethanol for 16 hours. After cooling, the solvent was evaporated and the crude brown mixture was purified by silica chromatography (1:9 methanol/dichloromethane). The still impure product was further recrystallized from methanol affording 70 mg pure product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07390808B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-5f81c07103d8477b9ab602dbda118848 |
| 出典メモ | uspto-grants-2008_06 |