참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| 반응물 | Thiourea | HCID 2723790 | — |
| 반응물 | HCID 178478442 | HCID 178478442 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178526719 | HCID 178526719 | — |
반응 단계
A mixture of 0.6 g (3.9 mmol) of 4-chloromethylimidazole and of an equimolar equivalent of thiourea (0.3 g) in 10 ml of ethanol is brought to reflux for 30 min. 5 ml of ethanol, 20 ml of water and 1.2 molar equivalents of 2-chloro-5-nitropyridine (0.74 g) in 5 ml of hot ethanol are added to this mixture. The light solution is cooled to 0°-10° C. in an ice bath and a solution of 0.49 g of sodium hydroxide in 10 ml of water is added dropwise under nitrogen at 0°-10° C. and then the mixture is stirred for a further 3 h at 21° C. The precipitate is collected, washed with water and chromatographed through silica gel with a mixture of chloroform and methanol (1-20%) to give the title compound, M.p.: 155°-156° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05559113 |
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| 출처 데이터셋 | uspto-grants-1996_09 |
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| ORD ID | ord-cba5ef77f7d54874a9bf356c2951b21a |
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| 출처 메모 | uspto-grants-1996_09 |
|---|