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HRID 535353作成日:2026年10月25日
2,3-Dichloropyridine → 6-(3-Chloropyridin-2-yl)-N-(6-(trifluoromethyl)pyridin-3-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine
https://huagongshe.com/reaction/535353
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Dichloropyridine | HCID 16988 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | N-(6-(Trifluoromethyl)pyridin-3-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine | HCID 59346451 | — |
| 溶媒 | dioxane N,N-dimethylacetamide | HCID 67000103 | — |
| 生成物 | 6-(3-Chloropyridin-2-yl)-N-(6-(trifluoromethyl)pyridin-3-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine | HCID 59346541 | 28% |
反応手順
N-(6-(Trifluoromethyl)pyridin-3-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (130 mg, 0.44 mmol) was dissolved in a mixture of dioxane/N,N-dimethylacetamide (4:1) (2 mL). To the mixture was added 2,3-dichloropyridine (98 mg, 0.66 mmol) and N,N-diisopropylethylamine (0.11 mL, 0.66 mmol). The mixture was heated at 150° C. in a Personal Chemistry microwave for 16 h. The solvents were removed under vacuum and the residue was dissolved in ethyl acetate and washed with sat. NaHCO3 and brine. The organic layer was dried over Na2SO4, filtered and evaporated to give a brown residue. The residue was purified using a gradient of ethyl acetate:hexane (0-100%) to give the desired compound as an off-white powder (50 mg, 28%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08859545B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-ca1bc9473e8e42aab5f96955a9aded9a |
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| 出典メモ | uspto-grants-2014_10 |
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