참여 물질
| 역할 | 이름 | HCID | 투입량 |
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| 반응물 | Stannous chloride dihydrate | HCID 61436 | — |
| 반응물 | 4,6-Dichloro-2-(methylthio)-5-nitropyrimidine | HCID 11345458 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 4,6-Dichloro-2-(methylsulfanyl)pyrimidin-5-amine | HCID 57742486 | 87% |
반응 단계
To a solution of 4,6-dichloro-2-methylsulfanyl-5-nitro-pyrimidine (1.0 g, 4.2 mmol) in EtOH (20 mL) was added SnCl2.2H2O (3.8 g, 17 mmol). The mixture was heated to 90° C. After 2 h, the reaction mixture was cooled and the solution was concentrated. The residue was treated with saturated (satd.) aqueous (aq.) NaHCO3 until pH 8. The resulting mixture was then extracted with EtOAc (3×100 mL). The combined organic extracts were dried, filtered, and concentrated. The residue was purified by FCC to afford a colorless solid (723 mg, 87%). MS (ESI): mass calcd. for C5H5Cl2N3S, 208.9; m/z found, 210.3 [M+H]+. 1H NMR ((CD3)2SO): 5.89 (s, 2H), 2.45 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09440978B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-54919978b75741c2a0c38f1762064981 |
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| 출처 메모 | uspto-grants-2016_09 |
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