HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 56849421, compound → HCID 66779373, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 56849421 | HCID 56849421 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ammonia methanol | HCID 21705897 | — |
| Product | HCID 66779373 | HCID 66779373 | 67% |
Reaction Steps
3-[2-(3,4,5-Trimethoxy-phenyl)-furo[3,2-b]pyridin-7-yl]-benzonitrile (0.067 mmol) is dissolved in methanol/NH3 (10%, 10 ml) and sponge nickel catalyst (70%, 0.1 g) is added. The mixture is hydrogenated at 5.6 bar at 50° C. for 15 h. The suspension is filtrated and the solvent removed in vacuo. The precipitate is suspended in diethylether and filtrated. The product is obtained after drying in vacuo as slight green solid (67% yield). HPLC (method A): Rt 2.41 min (purity 97.3%); LCMS (ESI+) (method E): Rt 1.527 min, M+H+ 391.1 m/z; 1H NMR (400 MHz, DMSO-d6) δ [ppm] 8.56 (d, J=4.8, 1H), 8.25 (s, 1H), 7.93 (d, J=7.1, 1H), 7.74 (s, 1H), 7.65-7.45 (m, 3H), 7.34 (s, 2H), 3.92 (s, 6H), 3.88 (s, 2H), 3.81-3.68 (m, 5H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09006440B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-b734f1b9d98a4fe7883e40b68cb1168c |
| Source note | uspto-grants-2015_04 |