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Methanesulfonic Acid → 6,8-difluoro-N-methyl-2,3,4,9-tetrahydro-1H-carbazol-3-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 2,4-Difluorophenylhydrazine hydrochloride | HCID 2733301 | — |
| 反応物 | 4-(Methylamino)cyclohexanone | HCID 20760632 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6,8-difluoro-N-methyl-2,3,4,9-tetrahydro-1H-carbazol-3-amine | HCID 12361823 | — |
反応手順
A solution of 3.5 g. of 4-methylaminocyclohexanone, 5.1 g. of 2,4-difluorophenylhydrazine hydrochloride, and 4 g. of methanesulfonic acid in 50 ml. of absolute ethyl alcohol was heated under reflux for four hours, cooled, and filtered. The resulting solids were washed with isopropanol and treated in chloroform with 10% potassium hydroxide solution. The chloroform extract was evaporated to dryness to give 3-(methylamino)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole, m.p. 135°-138°C., which was converted to the hydrochloride salt, m.p. >280°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03959309 |
| 出典データセット | uspto-grants-1976_05 |
| ORD ID | ord-a27f51d4920641bea5d26d4bf7cfe7b2 |
| 出典メモ | uspto-grants-1976_05 |