関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N-benzoyl-N'-(3-cyano-4,5-dimethyl-2-thienyl)thiourea | HCID 899430 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5,6-Dimethyl-2-(methylthio)thieno[2,3-d]pyrimidin-4-amine | HCID 1212338 | 89% |
反応手順
To a suspension of N-(3-cyano-4,5-dimethylthiophen-2-ylcarbamothioyl)-benzamide (Example 1a) (1.33 g, 4.22 mmol) in ethanol (25 mL) was added NaOH (2.0 N, 5.8 mL) at room temperature under nitrogen. After stirring at 100° C. under nitrogen for 0.5 h, the reaction mixture was cooled in an ice bath and MeI (0.8 mL) was added dropwise. After stirring for another 0.5 h, the resulting precipitate was collected by filtration, rinsed with water, 20% EtOH/H2O, and dried under vacuum to give the title compound (840 mg, 89%). 1H NMR (400 MHz, DMSO-d6) δ2.32 (s, 3H), 2.34 (s, 3H), 2.42 (s, 3H), 6.93 (bs, 2H). MS 226 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541421B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-994adbae99914d29a183882d3a020cdd |
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| 出典メモ | uspto-grants-2013_09 |
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