関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Aminothiophene-3-carboxamide | HCID 699495 | — |
| 反応物 | Potassium ethylxanthate | HCID 2735045 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-sulfanyl-3H,4H-thieno(2,3-d)pyrimidin-4-one | HCID 3603393 | 69.5% |
反応手順
2-Amino-thiophene-3-carboxlic acid amide (28.4 g, 0.2 mol) and potassium ethylxanthate (96 g, 3 eq) were mixed together and added to DMF (1000 mL). The resulting mixture was heated to 150° C. for about six hours. The solvent (DMF) was removed on the rotovap under high vacuum at 90° C. The residue was diluted with 600 mL of aqueous citric acid (5%) and cooled to 0° C. and stirred for about 30 minutes. The tan powder was filtered and dried overnight to give 25.6 g of the title compound ((M+H)+=185, M.P.>300° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07091347B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-9a87187d185b4d9390fcb9daeac9bc76 |
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| 出典メモ | uspto-grants-2006_08 |
|---|