HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 55028620, compound → HCID 59828903, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 55028620 | HCID 55028620 | — |
| Catalyst | Hydrochloric Acid | HCID 313 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 59828903 | HCID 59828903 | — |
Reaction Steps
Bubble nitrogen for 15 min into a solution of 4-[(2,2-dimethyl-propionylamino)-methyl]-benzonitrile (0.4 g, 1.85 mmol) in methanol (50 mL) with concentrated HCl (8 drops). Add 10% Pd/C (Degussa type E101, 40 mg) and submit the mixture to hydrogenation at atmospheric pressure overnight. Filter the catalyst through Celite® and concentrate in vacuo to obtain the hydrochloride salt of the title compound. Add saturated aqueous NaHCO3 and extract twice with EtOAc. Dry the combined organic extracts over MgSO4, filter and concentrate in vacuo to obtain the title compound as a yellow oil (315 mg, 77%). MS (ES+) m/z: 221 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680091B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-ee0a0aa1f1c248189e67ed5adc977e9b |
| Source note | uspto-grants-2014_03 |