関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzamidine | HCID 2332 | — |
| 反応物 | 2-Propenoic acid, 2-cyano-3-ethoxy-, ethyl ester | HCID 78943 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178510335 | HCID 178510335 | — |
反応手順
To a stirred solution of benzamidine (1.0 g, 8.32 mmol) in anhydrous DMF (20 mL ) was added Ethyl(ethoxymethylene)cyanoacetate (11) (1.41 g, 8.32 mmol, 1.0 equiv ) under argon at 0° C. The mixture was stirred at 0° C. for 2 h and increase to 105° C. for 60 h. The reaction mixture was then cooled to ambient temperature. The mixture was extracted with ethyl acetate (2×100 mL ). The combined organic extracts were washed with water (1×50 mL) and brine (1×50 mL), dried (Na2SO4), filtered, and evaporated in vacuo. The residue was washed with water (1×60 mL), dichloromethane (1×60 mL) then dried in the vacuum oven to obtain the light yellow solid as product (0.77 g, 47%). 1H-NMR (CD3CN) δ8.25 (s, 1H ), 8.06 (d, 2H ), 7.70 (t, 1H ), 7.61 (t, 2H). MS LC-MS (MH+=198).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07429584B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-e6425ac839a74fdbb7b9d89eec18c911 |
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| 出典メモ | uspto-grants-2008_09 |
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