HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 20482634, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 4,5-Dimethyl-1,2-phenylenediamine | HCID 76635 | — |
| Reactant | Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate | HCID 102624 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 20482634 | HCID 20482634 | 35% |
Reaction Steps
A solution of 1-benzyl-3-carbethoxy-4-piperidone (3 mmol, 784 mg) in xylene (20 mL) was treated at room temperature with 4,5-dimethyl-1,2-benzenediamine (3 mmol, 408.6 mg, 1 eq) and the suspension was stirred under reflux under argon overnight then further for 5 h. The mixture was concentrated under reduced pressure to give a brown residue, which was treated with ethyl acetate and a touch of methanol. Beige crystals formed from the brown solution and were filtered off and dried under reduced pressure (vacuum oven) to give the title compound (1.05 mmol, 350 mg, 35% yield). M+H 334.3.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288412B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-862a1be8f11b49e9a23092d0ee595196 |
| Source note | uspto-grants-2012_10 |