참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-(Ethoxymethylene)propanedinitrile | HCID 67152 | — |
| 반응물 | 2-Ethylphenylhydrazine Hydrochloride | HCID 2733209 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 5-Amino-1-(2-ethylphenyl)-1H-pyrazole-4-carbonitrile | HCID 12150558 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08809348B2 |
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| 출처 데이터셋 | uspto-grants-2014_08 |
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| ORD ID | ord-72ac73fcbd8a44bc9209e6e6d971e21c |
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| 출처 메모 | uspto-grants-2014_08 |
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