HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69092455, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 69060409 | HCID 69060409 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 69092455 | HCID 69092455 | 20% |
Reaction Steps
A mixture of benzyl 4-{6-[(phenylsulfonyl)amino]-2,3-dihydro-4H-chromen-4-ylidene}piperidine-1-carboxylate (500 mg, 1 mmol), ethanol (2 mL) and 6N hydrochloric acid (18 mL) is heated at reflux temperature for 2 hours, cooled to 0°-5° C., treated with 6N sodium hydroxide (14 mL) with cooling, then with saturated aqueous sodium carbonate to pH 9 and with chloroform. The organic phase is dried over MgSO4 and concentrated in vacuo. The resultant residue is crystallized from ethanol to afford the title compound as an off-white solid, 75 mg (20% yield), mp >230° C., identified by NMR and mass spectral analyses.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07534801B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-817d2ac46b0f4d299284cecfe7e1fe03 |
| Source note | uspto-grants-2009_05 |