関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Thiophenecarboxylic acid, tetrahydro-4-oxo-, methyl ester | HCID 98424 | — |
| 反応物 | Formamidine acetate | HCID 160693 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5,7-Dihydrothieno[3,4-d]pyrimidin-4-ol | HCID 136026346 | — |
反応手順
Commercially available 4-carbomethoxytetrahydro-3-thiophenone (5 g, 31.2 mmol) is dissolved in EtOH (284 mL). Formamidine acetate (22 g, 211 mmol) is then added followed by sodium ethoxide (45 mL, 121 mmol, 21% w/w) and the mixture is heated at 90° C. for 14 hours. Reaction is cooled to room temperature and concentrated to a residue which is absorbed onto silica and separated via FCC (0-10% Methanol:CH2Cl2) to give the title compound as a solid. MS (ESI) m/z 155.14 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541432B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-c65ef26a23c34fcbbc5714fcf01e5d96 |
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| 出典メモ | uspto-grants-2013_09 |
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