HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 131735534, compound → HCID 178501303, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 131735534 | HCID 131735534 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178501303 | HCID 178501303 | 100% |
Reaction Steps
A solution of the product of step 4 (480 mg, 0.686 mmol) in MeOH (9146 μl) and THF (4573 μl) was treated with a catalytic amount of 10% palladium on carbon (36 mg). The mixture was hydrogenated at 20 psi. After 2 hours LCMS showed >70% conversion. Hydrogenation was continued for another 2 h. LCMS showed >90% conversion. The mixture was diluted with ethyl acetate (50 mL) and the solids were removed by filtration. The filtrate was concentrated in rotavap and the residue was purified on a RediSep® (80 g) silica gel column (gradient: 0 to 50% ethyl acetate in hexanes) to give the title compound (420 mg, 0.684 mmol, 100% yield) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09328138B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-2d21f61c69284efab2edd83976ec593e |
| Source note | uspto-grants-2016_05 |