HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 18518277, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86585480 | HCID 86585480 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 18518277 | HCID 18518277 | 60.2% |
Reaction Steps
A mixture of ethyl (±)-10,11-dihydro-3-[3-(4-methylpyridin-2-ylamino)-1-propyloxy]dibenzo[b,f]oxepine-10-acetate (119 mg, 0.27 mmole) and 0.991 N NaOH (0.545 mL, 0.54 mmole) in absolute EtOH (2 mL) was warmed in an oil bath set at 45° C. After 20 hr, the reaction was concentrated on the rotavap, and the residue was dissolved in H2O (1.5 mL). The solution was filtered to remove insoluble material, and the filtrate was carefully neutralized by dropwise addition of 1.0 N HCl (0.54 mL, 0.54 mmole). The precipitate was collected and dried in high vacuum to afford the title compound (68 mg, 58%) as a white solid: MS (ES) m/e 418.9 (M+H)+. Anal. Calcd for C25H26N2O4. 0.45 HCl: C, 69.05; H, 6.13; N. 6.44. Found: C, 69.25; H, 6.27; N. 6.16.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06576643B2 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-aa437940d91545da9a30acdef2778f63 |
| Source note | uspto-grants-2003_06 |