HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 57656539, compound → HCID 57656471, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 57656539 | HCID 57656539 | — |
| Catalyst | Hydrochloric Acid | HCID 313 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 57656471 | HCID 57656471 | — |
Reaction Steps
Dissolve 4-(2-methyl-propane-2-sulfonylmethyl)-benzonitrile (300 mg, 1.26 mmol) in methanol (50 mL). Add concentrated HCl (10 drops), 10% Pd/C (Degussa type E101, 60 mg) and submit the mixture to hydrogenation at atmospheric pressure for 1 h. Filter over Celite® and wash with methanol. Concentrate the filtrate in vacuo to give the hydrochloride salt of the title compound as a solid that was washed with diethyl ether (366 mg, 87%). Partition the solid between saturated NaHCO3 and EtOAc and extract the aqueous phase twice with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo to give the title compound (195 mg, 74%). MS (ES+) m/z: 242 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08580780B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-620e253ed19449eeac973d6452e3f3df |
| Source note | uspto-grants-2013_11 |