참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,3-Dibromo-5,5-dimethylhydantoin | HCID 6479 | — |
| 반응물 | Sodium Phosphate, Dibasic | HCID 24203 | — |
| 반응물 | HCID 178461251 | HCID 178461251 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 178461196 | HCID 178461196 | — |
반응 단계
4,6-dichloro-3-[(trans-4-methylcyclohexyl)methyl]-3H-imidazo[4,5-c]pyridine (1 g, 3.35 mmol) was dissolved in THF (10 mL). Disodium hydrogen phosphate (1.43 g, 10.1 mmol) was added, and the reaction was warmed to 35° C. with stirring. 1,3-dibromo-5,5-dimethylhydantoin (1.15 g, 4.02 mmol) was added in 1 portion, and the reaction was continued with stirring at 35° C. After 45 minutes, the reaction was diluted with EtOAc (100 mL) and washed with aqueous NaHSO3 and brine. The organic layer was dried over Na2SO4, filtered, and concentrated. Purification of the residue on a silica gel column with 0 to 50% EtOAc/hexanes provided 2-bromo-4,6-dichloro-3-[(trans-4-methylcyclohexyl)methyl]-3H-imidazo[4,5-c]pyridine.
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-0c27f33962f648758fd76403fb149c44 |
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| 출처 메모 | uspto-grants-2014_09 |
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