HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 58303869, compound → HCID 58303860, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 58303869 | HCID 58303869 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 58303860 | HCID 58303860 | 94% |
Reaction Steps
A mixture of 17-4 (454 mg, 1.098 mmol) and Pd(OH)2/C in MeOH (0.5 mL NH3) was hydrogenated at ambient pressure for 30 min at 25° C., then the mixture was filtered through a plug of Celite and washed with EtOAc. The crude product was purified by column chromatography on silica gel eluting with Hexane/EtOAc (20%) to afford a white solid 17-5 in 94% yield (334 mg). 1H NMR (300 MHz, CDCl3) δ (ppm) 8.27 (br, 1H), 6.96 (dd, J=10.9, 8.8 Hz, 1H), 6.73 (s, 1H), 6.68 (dd, J=8.8, 3.3 Hz, 1H), 3.90 (t, J=5.2 Hz, 2H), 3.67 (s, 3H), 3.07 (t, J=5.5 Hz, 2H), 0.84 (s, 9H), 0.01 (s, 6H). LRMS: calc 323.2 and found: 324.2 [M+1].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08912220B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-4c4d5666850b457fbaa96414dcd163c5 |
| Source note | uspto-grants-2014_12 |