関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-(Ethoxymethylene)propanedinitrile | HCID 67152 | — |
| 反応物 | 2-Ethylphenylhydrazine Hydrochloride | HCID 2733209 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Amino-1-(2-ethylphenyl)-1H-pyrazole-4-carbonitrile | HCID 12150558 | — |
反応手順
A solution of 3.0 g (17.0 mmol) of 2-ethylphenylhydrazine hydrochloride and 2.12 g (17.0 mmol) of ethoxymethylenemalononitrile in 36 ml of ethanol is mixed with 7.1 ml (51.1 mmol) of triethylamine and heated at 60° C. until the reaction is complete according to a TLC check (about 30 min). For working up, the solvent is stripped off, and the residue is taken up in dichloromethane, washed with saturated sodium bicarbonate solution and dried over sodium sulphate. Concentration results in a crude product which is purified by column chromatography on silica gel (mobile phase dichloromethane with 0-10% methanol). 3.05 g (83.5% of theory) of the desired product are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08809348B2 |
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| 出典データセット | uspto-grants-2014_08 |
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| ORD ID | ord-72ac73fcbd8a44bc9209e6e6d971e21c |
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| 出典メモ | uspto-grants-2014_08 |
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