HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 59983191, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | HCID 59983189 | HCID 59983189 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59983191 | HCID 59983191 | 15.4% |
Reaction Steps
To a solution of 147B (400 mg, 1.3 mmol) in EtOAc (5 mL)-MeOH (15 mL) was bubbled with N2 for 15 min, then palladium hydroxide (20 weight % palladium on carbon) (200 mg) was added. The resulting suspension was subjected to hydrogenation under 80 psi of pressure for 16 h., then filtered. The filtrate was concentrated. The residue was chromatographed (silica gel) eluting with 20% EtOAc in hexane (100 mL), 50% EtOAc in hexane (100 mL), 100% ETOAc (100 mL), 5% MeOH in EtOAc (150 mL) to give title compound (62 mg, 15% yield) as a white foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07884113B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-b45e58bcf22f4395aec61152e1755915 |
| Source note | uspto-grants-2011_02 |