HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 24693813, compound → HCID 57656518, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 24693813 | HCID 24693813 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 57656518 | HCID 57656518 | 63.1% |
Reaction Steps
Charge a solution of 6-cyclohexylamino-nicotinonitrile (1.4 g, 7.1 mmol) in methanol (70 mL) and trifluoroacetic acid (5 mL) to a pressure vessel containing 10% Pd/C (Degussa type E101, 600 mg). Pressurize the vessel to 40 psi with hydrogen and stir for 2 h. Filter the mixture through Celite®, wash with warm ethanol, and dichloromethane. Concentrate the filtrate in vacuo. Purify the crude mixture by chromatography on silica gel eluting with dichloromethane/2M ammonia in methanol (99:1 to 90:10 gradient) to obtain the title compound (920 mg, 54%). MS (ES+) m/z: 206.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022062B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-e5528451159742f0a7ba4c6fd3e54d94 |
| Source note | uspto-grants-2011_09 |