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1-(Triphenylphosphoranylidene)acetone → Methyl 3-(3-oxo-1-butenyl)indole-6-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(Triphenylphosphoranylidene)acetone | HCID 15038 | — |
| 反応物 | methyl 3-formyl-1H-indole-6-carboxylate | HCID 735867 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Methyl 3-(3-oxo-1-butenyl)indole-6-carboxylate | HCID 53858282 | 17% |
反応手順
To a stirred solution of methyl 3-formylindole-6-carboxylate (368 mg) in 1,4-dioxane (10 ml) was added acetylmethylene triphenylphosphorane (1.15 g), and the mixture was stirred under reflux for 12 hours. The resulting mixture was evaporated in vacuo, redissolved with ethyl acetate and washed with 1N hydrochloric acid and brine. The organic phase was dried over sodium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel eluting with a mixture of chloroform and ethyl acetate (1:2) to give methyl 3-(3-oxo-1-butenyl)indole-6-carboxylate (75 mg) as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06358992B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-e5b7b3b9a0b94d1a9039241ad2e1a667 |
| 出典メモ | uspto-grants-2002_03 |