関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromo-2-butyne | HCID 2756862 | — |
| 反応物 | 2-bromo-1H-imidazole-4,5-dicarbonitrile | HCID 2779148 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-bromo-1-(2-butynyl)-1H-imidazole-4,5-dicarbonitrile | HCID 23070872 | — |
反応手順
69.8 g of potassium carbonate and 50 ml N,N-dimethylformamide solution of 74 ml of 1-bromo-2-butyne were added to a 520 ml N,N-dimethylformamide solution of 90.6 g of 2-bromo-1H-imidazole-4,5-dicarbonitrile [CAS No 50847-09-1], and the mixture was heated at 50° C. for 8 hours. 1 L of ethyl acetate and 500 ml of water were added to the solution, and the organic layer was washed twice with 500 ml of water and then with 500 ml of a saturated sodium chloride solution. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography. Thus, 48.0 g of the title compound was obtained from the fraction eluted with ethyl acetate-hexane (1:4).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07772226B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-56faf7657c0340b58029531e17688cc7 |
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| 出典メモ | uspto-grants-2010_08 |
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