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Phenylhydrazine → 5-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenylhydrazine | HCID 7516 | — |
| 反応物 | 2-(Ethoxymethylene)propanedinitrile | HCID 67152 | — |
| 反応物 | (1-Ethoxyethylidene)malononitrile | HCID 79450 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile | HCID 219858 | — |
反応手順
Into a 250-mL 3-necked round-bottom flask, was placed a solution of 1-phenylhydrazine (31.5 g, 291.67 mmol, 1.14 equiv) in ethanol (105 mL) at room temperature. To the resulting mixture was then added 2-(1-ethoxyethylidene)malononitrile (35 g, 257.35 mmol, 1.00 equiv) in several batches at room temperature. After about half of the addition was completed, the solution was carefully heated to boiling. After all the ethoxymethylene malononitrile was added, the resulting solution was heated to reflux for 4 hr. The resulting mixture was then cooled with a water/ice bath, and the solids were collected by filtration to yield 5-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822447B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-f135ab60af0c414f928bdb7fa3b2c11f |
| 出典メモ | uspto-grants-2014_09 |