関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 3-Cyanoindole | HCID 230282 | — |
| 反応物 | trans-N,N'-dimethyl-1,2-cyclohexanediamine | HCID 2733821 | — |
| 反応物 | Ethyl 2-bromoisonicotinate | HCID 3847769 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(3-Cyanoindol-1-yl)isonicotinic acid ethyl ester | HCID 58437311 | 30.1% |
反応手順
A mixture of 1H-indole-3-carbonitrile (0.1 g), 2-bromoisonicotinic acid ethyl ester (0.16 g), potassium phosphate (0.27 g), (1R,2R)-(−)-N,N′-dimethylcyclohexane-1,2-diamine (0.017 g), copper iodide (0.006 g) and toluene (0.7 mL) was stirred at 110° C. for 38 hours. The insoluble material was removed by filtration, and this filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: ethyl acetate/n-hexane=10/90 to 66/34) to give the title compound (0.061 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08829040B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-953e4f3bddfc4af7bead9475e160251d |
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| 出典メモ | uspto-grants-2014_09 |
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