HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 69251257, compound → HCID 59701475, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 69251257 | HCID 69251257 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ether hydrochloride | HCID 10953452 | — |
| Product | HCID 59701475 | HCID 59701475 | — |
Reaction Steps
(2-Chloro-3-trifluoromethyl-benzyl)-(2,2-diphenyl-ethyl)-[3-(4-chloro-3-nitro-phenoxy)-propyl]-amine (400 mg, 0.66 mmol) was hydrogenated over 10% Pd/C (40 mg) at 60 psi at room temperature in the presence of 1N HCl-Et2O (10 ml). After 24 h, the reaction mixture was filtered and concentrated in vacuo to give a heavy oil. HPLC purification of the crude amine (Phenomonex Luna Combi HTS, 5 micron C18, 275 mm×30 mm, 10% CH3CN— water gradient to 95% CH3CN) afforded the title compound as an oil. Treatment of the free base with 1N HCl-Et2O (excess), followed by filtration and isolation of the resulting precipitate gave the title compound as a brown solid, 18.5 mg (4.3%). MS (ESI) 572.5 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07365085B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-4caa8da2be294622b74682518db63313 |
| Source note | uspto-grants-2008_04 |