関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Chloro-5-methyl-pyridine | HCID 581393 | — |
| 反応物 | 5,6,7,8-Tetrahydropyrido[4,3-d]pyrimidin-4(3H)-one | HCID 135627628 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 溶媒 | Chloroform isopropyl alcohol | HCID 21906603 | — |
| 生成物 | 5,6,7,8-Tetrahydro-6-(5-methylpyridin-2-yl)pyrido[4,3-d]pyrimidin-4(3H)-one | HCID 135978957 | 48.5% |
反応手順
Into a 20 mL microwave tube was combined 5,6,7,8-tetrahydro-3H-pyrido[4,3-d]pyrimidin-4-one (0.280 g, 1.83 mmol), 2-chloro-5-methylpyridine (0.47 g, 3.7 mmol), 1,4-dioxane (2.5 mL), N,N-diisopropylethylamine (0.64 mL, 3.7 mmol) and N,N-dimethylacetamide (0.5 mL). 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 phase was washed with sodium bicarbonate and brine (1×50 mL), dried over sodium sulfate, and reduced in vacuo. The residue was purified by flash chromatography on silica gel (0-10% methanol/methylene chloride) to give a bright yellow solid (0.215 g, 47.9%). MS: 243.3 [M+1]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08653091B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-ee487f9731e740129df005f175727be1 |
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| 出典メモ | uspto-grants-2014_02 |
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