HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 27514272, compound → HCID 20670049, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 27514272 | HCID 27514272 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 20670049 | HCID 20670049 | 35.8% |
Reaction Steps
A solution of 2-methyl-3,5-dinitro-N-(tricyclo[3.3.1.13.7]dec-1-ylmethyl)-benzamide (Example 65) (2.66 g) in ethyl acetate (200 ml) was hydrogenated over palladium on carbon (10%, 0.5 g ) for 72 hours. The reaction mixture was then filtered through celite® and the residue washed with ethyl acetate. The filtrate and washings were combined and concentrated under reduced pressure to give a solid (0.8 g). This was purified by column chromatography over silica eluting with dichloromethane:ethanol (9:1). The product was further purified by treatment with charcoal in boiling ethanol followed by filtration and concentration to remove coloured impurities to give the title compound as a near colourless solid (0.58 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06303659B2 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-15221dfc62a9463c95a029d6bc446195 |
| Source note | uspto-grants-2001_10 |