HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 66745967, compound → HCID 66745861, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 66745967 | HCID 66745967 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol ethylacetate | HCID 21584252 | — |
| Product | HCID 66745861 | HCID 66745861 | 88.1% |
Reaction Steps
A suspension of 2-amino-6-(3,3-dimethylbut-1-ynyl)benzonitrile (Example 21c, 690 mg, 3.48 mmol) and 10% Pd/C (100 mg) in EtOAc/EtOH (1:1, 20 mL) was stirred under an atmosphere of H2 with a balloon at room temperature overnight. The Pd/C was removed by filtration, the filtrate was concentrated, and purified by chromatography on silica gel eluting with 20% EtOAc in hexanes to give the title compound as a light yellow oil (620 mg, 88%). 1H NR (400 MHz, DMSO-d6) δ 0.92 (s, 9H), 1.36-1.40 (m, 2H), 2.52-2.56 (m, 2H), 5.88 (s, 2H), 6.45 (d, J=7.6 Hz, 1H), 6.57 (d, J=7.6 Hz, 1H), 7.15 (t, J=8.0 Hz, 1H). MS 203 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09049878B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-ab6b0db4f8204234a402bdb2b43c014a |
| Source note | uspto-grants-2015_06 |