HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylindole → HCID 22462569, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylindole | HCID 11781 | — |
| Reactant | 4-Piperidone | HCID 33721 | — |
| Reactant | Hydrate;hydrochloride | HCID 21885828 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 22462569 | HCID 22462569 | 47% |
Reaction Steps
To a solution of 4-piperidone. H2O.HCl (50 g, 0.32 mol) in 100 ml of acetic acid and 150 ml of trifluoroacetic acid was added dropwise a solution of 1-methylindole (11.5 ml, 0.09 mol) in 100 ml of acetic acid at room temperature. After stirring for 1h the reaction mixture was concentrated (in vacuum , temp. ca. 30° C.), water was added , the mixture was made basic with potassium carbonate and extracted with ethyl acetate. The organic layer was separated, dried and purified by silica gel column chromatography (dichloromethane/methanol/ammonium hydroxide =84/15/1) to give 9 g (47%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06391896B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-fba3650eed98432f8a885c2928c2198a |
| Source note | uspto-grants-2002_05 |