참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1,1,1-Trifluoro-2-nitroethane | HCID 522762 | — |
| 반응물 | N-[(6-Chloro-3-pyridinyl)methyl]-1,2-ethanediamine | HCID 10997737 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2-Chloro-5-{[2-(nitromethylidene)imidazolidin-1-yl]methyl}pyridine | HCID 180957 | 70.1% |
반응 단계
5 g (26.9 mmol) of N-(2-chloro-5-pyridylmethyl)ethylene-diamine and 11.7 g (84.6 mmol) of potassium carbonate are placed in 40 ml of methanol. A solution of 3.64 g (28.2 mmol) of 1,1,1-trifluoro-2-nitro-ethane in 20 ml of methanol is added dropwise at 5° C. to 10° C. within 30 minutes. After the addition is complete, the mixture is stirred for 5 hours at 20° C. The mixture is then concentrated by removal of the solvent by distillation in vacuo, and the residue is taken up in methylene chloride, washed with a small amount of water, dried, concentrated and recrystallized from methanol. 4.6 g (70.1% of theory) of 1-(2-chloro-5-pyridylmethyl)-2-(nitromethylene)-imidazoline of a melting point of 160° C. to 161° C. are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04767864 |
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| 출처 데이터셋 | uspto-grants-1988_08 |
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| ORD ID | ord-49abe6dc727b45378bf0d7da4fc51e53 |
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| 출처 메모 | uspto-grants-1988_08 |
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