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Cesium carbonate → 5-diethylcarbamoylmethoxy-1H-indole-2-carboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Chloro-N,N-diethylacetamide | HCID 16844 | — |
| 反応物 | Ethyl 5-hydroxy-1H-indole-2-carboxylate | HCID 90677 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-diethylcarbamoylmethoxy-1H-indole-2-carboxylic acid ethyl ester | HCID 69586796 | 32.7% |
反応手順
A mixture of 5-hydroxy-1H-indole-2-carboxylic acid ethyl ester (1 g, 5 mmol), 2-chloro-N,N-diethylacetamide (1 mL, 7.5 mmol) and cesium carbonate (5 g, 15 mmol) in dimethylformamide (10 mL) was stirred at room temperature for 6 hours. The reaction was diluted with ethyl acetate (160 mL), washed with water (5×50 mL) and brine, dried and concentrated. The residue was recrystallized from ethyl acetate and hexane to give 0.52 g of 5-diethylcarbamoylmethoxy-1H-indole-2-carboxylic acid ethyl ester as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706709B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-d30592fe0a654af78f0c4e54d59a10d2 |
| 出典メモ | uspto-grants-2004_03 |