HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 59485041, compound → HCID 59485088, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 59485041 | HCID 59485041 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59485088 | HCID 59485088 | 32.1% |
Reaction Steps
To the ethyl acetate (6 mL) solution of N-benzyl-1-{5-[4-(4-methoxyphenyl)piperazin-1-yl]-2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran-2-yl}-N-methylmethaneamine (190 mg, 0.380 mmol) synthesized in Example 103, 10%-palladium carbon (comprising 50% moisture, 70 mg) was added, and then the mixture was stirred at room temperature for 15 hours under hydrogen atmosphere. The reaction mixture was filtered to remove the palladium carbon, and the filtrate was concentrated under reduced pressure. The residue was purified by basic silica gel chromatography (hexane-ethyl acetate 95:5-50:50), and recrystallized from ethyl acetate-hexane to obtain the title compound 50 mg (yield 32%). Melting point was 107 to 113° C. (ethyl acetate-hexane).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288390B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-4b0bf5f63cc947d5a595b25ace02284a |
| Source note | uspto-grants-2012_10 |