HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67163658, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 57439209 | HCID 57439209 | — |
| Catalyst | Ethanol | HCID 702 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67163658 | HCID 67163658 | 51% |
Reaction Steps
To a solution of 2-(1-methylpiperidin-4-yloxy)-7-(piperidin-4-yloxy)-fluoren-9-one (81 mg, 0.21 mmol; Example 24A) in EtOAc (10 mL) containing a few drops of ethanol was added a solution of HCl in dioxane (4 M, 335 μL, 1.34 mmol; Aldrich). After stirring the mixture for 2 h, the solid was collected by filtration and recrystallized from hot EtOH-EtOAc to afford the title compound (50 mg, 0.11 mmol, 51% yield): 1H NMR (300 MHz, CD3OD) δ ppm 1.97-2.11 (m, 3H), 2.11-2.27 (m, 4H), 2.92 (s, 3H), 3.18-3.30 (m, 4H), 3.35-3.47 (m, 4H), 4.72-4.81 (m, 2H), 7.14 (dd, J=8, 2 Hz, 2H), 7.22 (d, J=2 Hz, 2H), 7.50 (d, J=8 Hz, 2H); MS (DCl/NH3) m/z 393 (M+H)+; Anal. C24H28N2O3.2HCl: C, H, N.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07365193B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-558e6ec9a43f4ca8b6e059efd16e55f9 |
| Source note | uspto-grants-2008_04 |