関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | Methyl 3-amino-2-thiophenecarboxylate | HCID 89652 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3H,4H-thieno[3,2-d]pyrimidin-4-one | HCID 135417422 | 26% |
反応手順
A mixture of methyl 3-aminothiophene-2-carboxylate (1 g, 6.3 mmol) and formamide (2 g) is heated at 240° C. for 10 min. Upon cooling a precipitate appeared. It is dissolved in EtOH and filtered. The filtrate is concentrated under reduced pressure and the residue is purified by silica gel chromatography eluting with 10% MeOH in CH2Cl2 to yield 3H-thieno[3,2-d]pyrimid-4-one (249 mg, 26%) as a solid. 1H NMR (DMSO) δ 12.61 (1H, brs), 8.20 (1H, s), 8.17 (1H, d, J=5 Hz), 7.42 (1H, d, J=5 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06713484B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-21551590b0f94b3e97926eeaf14e009e |
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| 出典メモ | uspto-grants-2004_03 |
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