HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 67282662, compound → HCID 67281391, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 67282662 | HCID 67282662 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Acetonitrile--water (1/1) | HCID 18373917 | — |
| Product | HCID 67281391 | HCID 67281391 | — |
Reaction Steps
A solution of 32 (113 mg, 0.16 mmol) in MeOH (15 mL) was treated with 10% Pd/C (wet, 151 mg) and pressurized under H2 atmosphere (50 psi) using a Parr apparatus. After 2.5 h, the reaction mixture was filtered through a filter disc (Acrodisc-PSF-0.45 μM) and rinsed with MeOH. The filtrate was concentrated to afford the crude amine 33 which was diluted with ACN/H2O containing 0.1% HOAc and purified by reverse phase HPLC (2″ Dynamax® C18, 10% ACN/H2O to 100% ACN over 30 min). The product-containing fractions were combined, frozen, and lyophilized to afford 33 as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481495B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-0fa54716407442a0900014aa474ef43b |
| Source note | uspto-grants-2013_07 |