HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 10155946, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 54434818 | HCID 54434818 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 10155946 | HCID 10155946 | 65% |
Reaction Steps
A mixture of ethyl (±)-8-[3-(2-pyridylamino)-1-propyloxy]-3-oxo-2,3,4,5-tetrahydro-1H-2-benzazepine-4-acetate (0.7 g, 2 mmol), lithium hydroxide monohydrate (0.12 g, 3 mmol), 5 mL THF (5 mL), H2O (5 mL), and MeOH (2 mL) was stirred at room temperature for 18 hr, then was then concentrated. The residue was partitioned between ethyl acetate and water, and the layers were separated. The aqueous phase was cautiously brought to pH 4 with 3 N HCl and allowed to stand. The resulting crystals were collected by filtration and dried to give the title compound (0.4 g, 65%) as a tan solid: MS m/e 370.4 (M+H)+. Anal. Calcd for C20H23N3O4.0.25 H2O: C, 64.25; H, 6.34; N, 11.24. Found: C, 64.02; H, 6.37; N, 11.20.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06825188B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-52c3b727619e4202a48f31eb720185ca |
| Source note | uspto-grants-2004_11 |