HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 90112662, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 90112022 | HCID 90112022 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 90112662 | HCID 90112662 | 99.3% |
Reaction Steps
A solution of 5-(5-fluoro-4-methoxy-6-methyl-pyrimidin-2-yl)-6a-pyrazin-2-yl-3,3a,4,6-tetrahydro-1H-pyrrolo[3,4-c]isoxazole (0.92 g, 2.77 mmol) in ethanol (40 mL) is hydrogenated at 50 psi in the presence of Raney nickel (as a slurry in water) (2.7 g, 45.54 mmol) for 5 hours using a PARR hydrogenator. Methanol is added and the catalyst removed by filtration through a pad of diatomaceous earth. The diatomaceous earth pad is washed with methanol. The combined filtrates are concentrated under reduced pressure to give the title compound (0.92 g, 99%). ES/MS (m/e): 335 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09328124B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-66004be7a04d4c919cda6d874110987d |
| Source note | uspto-grants-2016_05 |