HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 58550791, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 58551780 | HCID 58551780 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58550791 | HCID 58550791 | 50.3% |
Reaction Steps
tert-Butyl 4-[1-(2-fluorophenyl)imidazol-2-yl]-4-hydroxy-piperidine-1-carboxylate (294 mg, 0.81 mmol) and K2CO3 (337 mg, 2.44 mmol) were heated at 110° C. for 16 h in DMF (5 mL). The solvent was evaporated and the resulting material was partitioned between dichloromethane and water. The organics were separated and washed with brine, dried over sodium sulfate and evaporated. The crude material was purified by column chromatography (0-50% ethyl acetate in hexanes) to give tert-butyl spiro[imidazo[2,1-c][1,4]benzoxazine-4,4′-piperidine]-1′-carboxylate (139 mg, 50%). ESI-MS m/z calc. 341.2, found 342.3 (M+1)+. Retention time 1.31 minutes (3 min run).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09365588B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-3cf54bcb61514d96ba194d57b072abd5 |
| Source note | uspto-grants-2016_06 |