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1-Methoxyethanol → 1-Methyl-7-benzoyloxindole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Methoxyethanol | HCID 3015637 | — |
| 反応物 | 3-Chloro-1-methyl-7-benzoylindole | HCID 23342675 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Phosphoric Acid | HCID 1004 | — |
| 生成物 | 1-Methyl-7-benzoyloxindole | HCID 20189472 | — |
反応手順
A solution of 46 grams (0.17 mol) of 3-chloro-1-methyl-7-benzoylindole in 250 ml of methoxy-ethanol and 60 ml of 70% phosphoric acid was heated at reflux under a nitrogen atmosphere for 5 hours. The solution was then cooled and diluted with 1.5 liters of water. The organic materials were extracted with methylene chloride and concentrated. The concentrated extract was chromatographed on silica gel and the product eluted with isopropyl ether. The residue obtained crystallized upon standing and was recrystallized from isopropyl alcohol to give 8.9 grams of 1-methyl-7-benzoylindolin-2-one, having a m.p. of 89°-90.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04221716 |
| 出典データセット | uspto-grants-1980_09 |
| ORD ID | ord-6b2b40f587964fccaca9e2784d9ad6cf |
| 出典メモ | uspto-grants-1980_09 |