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Methanesulfonic Acid → 3-(Isobutylamino)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole 3-(Acetamido)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | N-(4-Oxocyclohexyl)acetamide | HCID 538565 | — |
| 反応物 | 2,4-Difluorophenylhydrazine hydrochloride | HCID 2733301 | — |
| 反応物 | 3-(Acetamido)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole | HCID 12891807 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-(Isobutylamino)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole 3-(Acetamido)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole | HCID 23470518 | — |
反応手順
A solution of 15.5 g. of 4-acetamidocyclohexanone, 18 g. of 2,4-difluorophenylhydrazine hydrochloride and 10 g. of methanesulfonic acid in 200 ml. of absolute ethyl alcohol was heated under reflux for two hours, cooled, filtered, and the filtrate was evaporated to dryness under reduced pressure. The residual oil was triturated with water and the resulting solid was collected by filtration, triturated with ether, and recrystallized by dissolving in methanol, adding toluene, and evaporating the methanol to give 8.5 g. of 3-(acetamido)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole, m.p. 179°-183° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04257952 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-7777562742ca4dd4bc933cd89e1f6c06 |
| 出典メモ | uspto-grants-1981_03 |