참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | Dimethylacetamide | HCID 31374 | — |
| 반응물 | 2-Chloro-5-methyl-pyridine | HCID 581393 | — |
| 반응물 | 5,6,7,8-Tetrahydropyrido[4,3-d]pyrimidin-4(3H)-one | HCID 135627628 | — |
| 용매 | Chloroform isopropyl alcohol | HCID 21906603 | — |
| 생성물 | 5,6,7,8-Tetrahydro-6-(5-methylpyridin-2-yl)pyrido[4,3-d]pyrimidin-4(3H)-one | HCID 135978957 | 48.5% |
반응 단계
Into a 20 ml microwave tube was combined 5,6,7,8-Tetrahydro-3H-pyrido[4,3-d]pyrimidin-4-one (0.280 g, 0.00183 mol), 2-chloro-5-methylpyridine (0.47 g, 0.0037 mol), 1,4-dioxane (2.5 mL, 0.032 mol) N,N-diisopropylethylamine (0.64 mL, 0.0037 mol) and N,N-dimethylacetamide (0.5 mL, 0.005 mol). The mixture was heated via microwave at 150° C. for 4 hours. The mixture was reduced in vacuo and taken up in chloroform:IPA (3:1) (50 ml). The organic was washed with sodium bicarbonate and brine (1×50 ml), dried over sodium sulfate, and reduced in vacuo. The mixture was purified by flash chromatography on silica gel using a methylene chloride:methanol (0-10%) gradient. The combined pure fractions were reduced in vacuo to yield a bright yellow solid (0.215 g, 47.9%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07745451B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-f5fb789182c64475b71a7962bb9ce2e6 |
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| 출처 메모 | uspto-grants-2010_06 |
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