HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methyl-4-piperidone → HCID 59455254, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methyl-4-piperidone | HCID 74049 | — |
| Reactant | (2,4-Dichlorophenyl)hydrazine monohydrochloride | HCID 2723905 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 59455254 | HCID 59455254 | — |
Reaction Steps
2,4-Dichlorophenyl 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 15 min., followed by heating at 80° C. for 14 h. After completion of the reaction, as monitored by LCMS, the solvent is removed in vacuo, basified with saturated aq. NaHCO3 and extracted with EtOAc. The organic layer is separated, dried over anhydrous sodium sulfate and concentrated. The resulting crude product is purified by column chromatography to afford 6,8-dichloro-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-f6a5873844b5495d8dc4789e58cd405b |
| Source note | uspto-grants-2014_12 |