참여 물질
| 역할 | 이름 | HCID | 투입량 |
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| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Butanenitrile, 3-imino- | HCID 70698 | — |
| 반응물 | 4-Hydrazinyl-6-(methylthio)pyrimidine | HCID 13519855 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-Methyl-2-(6-methylsulfanyl-pyrimidin-4-yl)-2H-pyrazol-3-ylamine | HCID 59173368 | — |
반응 단계
The mixture of (6-Methylsulfanyl-pyrimidin-4-yl)-hydrazine (1.0 g, 6.4 mmol), 3-Imino-butyronitrile (1.1 g, 12.8 mmol), and ethanol (30 mL) is heated to 85° C. for overnight. The reaction mixture is then cooled to room temperature, condensed, and treated with 75 mL ethyl acetate. The reaction mixture is partitioned between ethyl acetate and aqueous layer. The organic layer is dried over Na2SO4 and concentrated. The crude product is purified by ISCO chromatography eluting with ethyl acetate in hexanes from 10% to 80% to afford 5-Methyl-2-(6-methylsulfanyl-pyrimidin-4-yl)-2H-pyrazol-3-ylamine: 1H NMR 400 MHz (d6-DMSO) δ 8.72 (s, 1H), 7.53 (s, 1H), 6.90 (s, 1H), 5.26 (s, 1H), 2.57 (s, 3H), 2.08 (s, 3H); MS m/z 222.07 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08202876B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-e8f9c9326c874781be6fe58dad94815f |
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| 출처 메모 | uspto-grants-2012_06 |
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