참여 물질
| 역할 | 이름 | HCID | 투입량 |
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| 반응물 | HCID 178463362 | HCID 178463362 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | HCID 178463350 | HCID 178463350 | — |
반응 단계
Crude tert-butyl (2,6-dichloro-3-((1-(trans-4-methylcyclohexyl)ethyl)amino)pyridin-4-yl)carbamate (70 g, 0.17 mol) was dissolved in a solution of HCl in dioxane (550 mL, 4 mol/L). The mixture was heated to 50° C. for 12 h. TLC (petroleum ether/ethyl acetate=5:1) showed the reaction was complete. White solid appeared. The solvent was removed under reduced pressure. The residue was washed with methyl tertiary butyl ether to give crude 2,6-dichloro-N3-(1-(trans-4-methylcyclohexyl)ethyl)pyridine-3,4-diamine, which was used for the next step without further purification. 1H NMR (400 MHz, DMSO-d6) δ: 6.63 (s, 1H), 3.16-3.13 (m, 1H), 1.84-1.76 (m, 2H), 1.67 (bs, 2H), 1.39 (bs, 1H), 1.25 (bs, 1H), 1.10-0.96 (m, 5H), 0.89-0.81 (m, 5H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08846657B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-dd5d5f61dc314b0683c88dfb9d7fa51a |
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| 출처 메모 | uspto-grants-2014_09 |
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