HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 7-chloro-5-(2-cyclohexylethyl)-2,3,4,5-tetrahydro-2-methyl-1H-pyrido[4,3-b]indole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | (2-Bromoethyl)cyclohexane | HCID 15440 | — |
| Reactant | m-Chlorophenylhydrazine hydrochloride | HCID 75331 | — |
| Reactant | 1-Methylpiperidin-4-one hydrochloride | HCID 12210057 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 7-chloro-5-(2-cyclohexylethyl)-2,3,4,5-tetrahydro-2-methyl-1H-pyrido[4,3-b]indole | HCID 57876276 | — |
| Product | 9-chloro-5-(2-cyclohexylethyl)-2,3,4,5-tetrahydro-2-methyl-1H-pyrido[4,3-b]indole | HCID 57876332 | — |
Reaction Steps
Preparation of the title compounds was carried out according to General Method 8. 3-Chlorophenylhydrazine hydrochloride (5 g, 27.9 mmol), 1-bromo-2-cyclohexylethane (4.37 ml, 27.9 mmol), triethyl amine (11.66 ml, 83.7 mmol) and N-methyl-4-piperidone hydrochloride (4 g, 27.9 mmol) were combined in ethanol (30 ml) to obtain 9-chloro-5-(2-cyclohexylethyl)-2,3,4,5-tetrahydro-2-methyl-1H-pyrido[4,3-b]indole and 7-chloro-5-(2-cyclohexylethyl)-2,3,4,5-tetrahydro-2-methyl-1H-pyrido[4,3-b]indole after on purification on silica gel (230-400 mesh) chromatography eluting with acetone-hexane gradient. The free base was converted into its oxalate salt by treatment of oxalic acid (1 equiv.) in anhydrous THF.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338408B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-3af1ac6624c14d4fbe073fe1bc2253fd |
| Source note | uspto-grants-2012_12 |