참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | N-benzoyl-N'-(3-cyano-4,5-dimethyl-2-thienyl)thiourea | HCID 899430 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 5,6-Dimethyl-2-(methylthio)thieno[2,3-d]pyrimidin-4-amine | HCID 1212338 | 89% |
반응 단계
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+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08541421B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-994adbae99914d29a183882d3a020cdd |
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| 출처 메모 | uspto-grants-2013_09 |
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