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Cesium carbonate → ethyl 1-(4-methoxybutyl)-7-oxo-4,5,6,7-tetrahydro-1H-indole-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Ethyl 7-oxo-1,4,5,6-tetrahydroindole-2-carboxylate | HCID 848532 | — |
| 反応物 | 4-Methoxybutyl methanesulfonate | HCID 11687006 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | ethyl 1-(4-methoxybutyl)-7-oxo-4,5,6,7-tetrahydro-1H-indole-2-carboxylate | HCID 58355155 | 85.3% |
反応手順
A solution of ethyl 7-oxo-4,5,6,7-tetrahydro-1H-indole-2-carboxylate (207 mg), 4-methoxybutyl methanesulfonate (273 mg) and cesium carbonate (652 mg) in N,N-dimethylacetamide (10 ml) was stirred at 60° C. for 15 hr. After cooling to room temperature, the reaction mixture was diluted with water and extracted with ethyl acetate (10 ml×2). The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate-hexane (5:95-3:7) was concentrated under reduced pressure to give the object product (250 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08664380B2 |
| 出典データセット | uspto-grants-2014_03 |
| ORD ID | ord-409c4f51f5724c9799bca2071fd10c94 |
| 出典メモ | uspto-grants-2014_03 |