HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 19769405, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 9949784 | HCID 9949784 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19769405 | HCID 19769405 | 79.6% |
Reaction Steps
A mixture of 2,3-dihydro-2-(1-methyl-piperidin-4-yl)-6-nitro-1H-benz[de]isoquinoline-1,3-dione (11.5 g; 33.9 mmol), prepared as in Example 3, in water (150 mL) and methanol (350 mL) was hydrogenated at atmospheric pressure over 10% Pd/C catalyst (1.4 g) for 5 hours. The catalyst was removed by filtration and the filtrate concentrated to a small volume. Isopropanol was added and the solution concentrated. Isopropanol was again added to the residue and the solution reconcentrated. The residue was swirled in ethanol and ether and the solid residue collected on a Buechner funnel. Drying under vacuum gave 6-amino-2,3-dihydro-2-(1-methylpiperidin-4-yl)-1H-benz[de]isoquinoline-1,3-dione (9.34 g; 27.0 mmol), m.p 345°-348° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05202318 |
| Source dataset | uspto-grants-1993_04 |
| ORD ID | ord-28640b02a1cc4907ab870b1b3a6aa169 |
| Source note | uspto-grants-1993_04 |