HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 18518335, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86585481 | HCID 86585481 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 18518335 | HCID 18518335 | 68.5% |
Reaction Steps
A mixture of ethyl (±)-10,11-dihydro-3-[2-[6(methylamino)pyridin-2-yl]-1-ethoxy]dibenzo[b,f]oxepine-10-acetic acid (0.26 mmole) and 0.991 N NaOH (0.525 mL, 0.52 mmole) in absolute EtOH (2 mL) was warmed in an oil bath set at 50° 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. The precipitate was collected and dried in high vacuum to afford the title compound (72 mg, 30% for 2 steps) as an off-white solid: MS (ES) m/e 405.0 (M+H)+. Anal. Calcd for C24H24N2O4.1.25HCl. 0.25H2O: C, 63.42; H, 5.71; N, 6.16. Found: C, 63.35; H, 5.9; N, 6.16.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06576643B2 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-0a5f3a382fb349839efa15dd06629ef8 |
| Source note | uspto-grants-2003_06 |