HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methyl-4-piperidone → 8-chloro-6-fluoro-2-methyl-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]indole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methyl-4-piperidone | HCID 74049 | — |
| Reactant | (4-Chloro-2-fluorophenyl)hydrazine hydrochloride | HCID 2782933 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 8-chloro-6-fluoro-2-methyl-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]indole | HCID 59455038 | — |
Reaction Steps
4-Chloro-2-fluorophenyl hydrazine hydrochloride (1 equiv.) is taken in 7% sulfuric acid in 1,4-dioxan. N-Methylpiperidine-4-one (0.76-1.4 equiv.) is added and the contents are stirred at RT for 10 min. The reaction mixture is then stirred at 100° C. for 6 h. The reaction is monitored by TLC and LCMS. After completion of the reaction, the reaction mixture is concentrated and then slowly quenched with aq. NaHCO3 solution, followed by extraction with EtOAc. The organic layer is dried over anhydrous sodium sulfate and evaporated to dryness. The crude product is purified by column chromatography to afford 8-chloro-6-fluoro-2-methyl-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]indole.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08907097B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-284a8d4f2e64428ba6bfcb4c5355aa45 |
| Source note | uspto-grants-2014_12 |