HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 67243837, compound → HCID 25026779, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 67243837 | HCID 67243837 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 25026779 | HCID 25026779 | — |
Reaction Steps
A solution of the free base of 6′-fluoro-4′,9′-dihydro-N-(4-methoxybenzyl)-4-benzyl-spiro[cyclohexane-1,1′(3′H)-pyrano[3,4-b]indol]-4-amine citrate (200 mg, 0.4 mmol) in tetrahydrofuran (20 ml) and methanol (20 ml) was mixed with 10% palladium on activated carbon (40 mg) and hydrogenated for 7 h under 3 bar and at 40° C. Then the reaction mixture was filtered through a pleated filter, the filter residue was washed with methanol and the filtrate was concentrated to small volume under vacuum. The crude product (186 mg) was purified by flash chromatography (20 g, 21×2 cm) with methanol. Yield: 136 mg (64%), beige-coloured solid. Melting point 198-205° C. (decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07960404B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-e7944de3426948a6977ace355ccef918 |
| Source note | uspto-grants-2011_06 |