HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → 6966-30-9
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Reactant | HCID 178472165 | HCID 178472165 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 6966-30-9 | HCID 227287 | 209.2% |
Reaction Steps
With stirring, a mixture of 221 g of ethyl 2-oximinobenzoylacetate (ethyl 2-oximino-3-oxo-3-phenylpropionate), 500 g of acetic anhydride, 50 g of glacial acetic acid and 20 g of a Pd/C catalyst (EF 101 R/W 51% H2O, sold by Degussa) is hydrogenated under normal pressure at 60° C. over 4 hours. The hydrogen uptake is 40 l. Afterwards the reactor is made inert with N2, flushed with nitrogen and the catalyst is removed by filtration. The filtrate is subsequently concentrated under reduced pressure on a rotary evaporator to give a residue (259.3 g), which is recrystallised from 200 ml of isopropanol/500 ml of petroleum ether.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05322964 |
| Source dataset | uspto-grants-1994_06 |
| ORD ID | ord-e892b295ae4e4c9cb1ea0185f90691bf |
| Source note | uspto-grants-1994_06 |