関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Chlorosulfonyl isocyanate | HCID 70918 | — |
| 反応物 | 6-(Trifluoromethoxy)-1H-indole | HCID 22048958 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Ethyl-6-trifluoromethoxyindole-3-carbonitrile | HCID 59425835 | 86% |
反応手順
To a solution of 6-trifluoromethoxyindole (2.68 g, 13.3 mmol) in dry DMF (10 mL) at 0° C., is added chlorosulfonylisocyanate (2.35 g, 1.44 mL, 16.6 mmol). The mixture is then brought to room temperature slowly and stirred for 1 h. The mixture is poured into ice (100 mL) and stirred for 1 h. The precipitate is collected by filtration and washed thoroughly with water and dried in vacuo, which is then dissolved in DMF (15 mL). To the solution is added K2CO3 and EtI (2.59 g, 1.34 mL, 16.6 mmol), and the mixture is stirred at 50° C. overnight. It is then poured into ice-water (200 mL). The precipitate is collected by filtration and washed with water, dried in air and purified by chromatography (silica gel, DCM) to furnish 1-ethyl-6-trifluoromethoxyindole-3-carbonitrile (2.90 g, 86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07781478B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-57889372f990460cb4e04f91ccbcdc83 |
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| 出典メモ | uspto-grants-2010_08 |
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