HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 131735533, compound → HCID 178501304, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 131735533 | HCID 131735533 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178501304 | HCID 178501304 | 93.4% |
Reaction Steps
A solution of the product of step 4 (870 mg, 1.280 mmol) in MeOH (8532 μl) and THF (4266 μl) was treated with a catalytic amount of 10% palladium on carbon (68 mg). The mixture was hydrogenated at 30 psi. After 6 hours LCMS showed complete reaction. The mixture was diluted with dichloromethane (50 mL) and the solids were removed by filtration. The filtrate was concentrated in rotavap and the residue was purified on a gold cap RediSep® (80 g) silica gel column (gradient: 0 to 40% ethyl acetate in hexanes) to give the title compound (710 mg, 1.196 mmol, 93% 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-9a8970f9e57a453ea27055155dcc058f |
| Source note | uspto-grants-2016_05 |