関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Ethyl 4-cyanobenzoate | HCID 81589 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | HCID 178506865 | HCID 178506865 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | ethyl 4-(N,N-dimethylamidino)benzoate | HCID 22631319 | — |
反応手順
To a tetrahydrofuran solution of 2M dimethylamine, 2.3M hexane solution of hexyllithium was slowly added over a period of at least three (3) hours while maintaining the temperature at between −8° C. and −12° C. This solution was added to the tetrahydrofuran solution of ethyl-4-cyanobenzoate (F) while maintaining the temperature between −8° C. and −12° C. The completion of the reaction was confirmed by HPLC, and the solution temperature was adjusted to between −8° C. and 3° C. The reaction mixture was slowly added to the cold solution of aqueous sodium bicarbonate solution and the desired ethyl-4-(N,N-dimethylcarbamimidoyl)benzoate (G) was extracted with ethyl acetate. The ethyl acetate layer was dried, filtered and evaporated under vacuum to afford ethyl-4-(N,N-dimethylcarbamimidoyl)benzoate (G) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08987463B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-6b8c5798f8b844fb8f5d4e50764ea7c2 |
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| 出典メモ | uspto-grants-2015_03 |
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