HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 3-(Isobutylamino)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole 3-(Acetamido)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | N-(4-Oxocyclohexyl)acetamide | HCID 538565 | — |
| Reactant | 2,4-Difluorophenylhydrazine hydrochloride | HCID 2733301 | — |
| Reactant | 3-(Acetamido)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole | HCID 12891807 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 3-(Isobutylamino)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole 3-(Acetamido)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole | HCID 23470518 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04172834 |
| Source dataset | uspto-grants-1979_10 |
| ORD ID | ord-f6a00a5477084bccbf14ac30871d8178 |
| Source note | uspto-grants-1979_10 |