HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,5-bis-(1,1-dimethylethyl)-4-hydroxy-N-[(4-nitrophenyl)methyl]-benzamide → 3,5-bis-(1,1-dimethylethyl)-4-hydroxy-N-[(4-aminophenyl)methyl]-benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,5-bis-(1,1-dimethylethyl)-4-hydroxy-N-[(4-nitrophenyl)methyl]-benzamide | HCID 21918554 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Palladium | HCID 23938 | — |
| Solvent | Dichloromethane ethanol | HCID 21584144 | — |
| Product | 3,5-bis-(1,1-dimethylethyl)-4-hydroxy-N-[(4-aminophenyl)methyl]-benzamide | HCID 21918612 | 62.1% |
Reaction Steps
In a 250 ml Parr flask, 2.85 g (7.4 mmoles) of 3,5-bis-(1,1-dimethylethyl)-4-hydroxy-N-[(4-nitrophenyl)methyl]-benzamide is dissolved in 30 ml of an absolute ethanol/dichloromethane mixture (1/1) in the presence of 10% Pd/C. The mixture is agitated under 20 PSI of hydrogen, at 30° C., for one hour. After filtration on celite, the filtrate is concentrated under vacuum. The evaporation residue crystallizes spontaneously. It is left to rest overnight, the crystals are filtered out and rinsed with a mixture of diethyl ether (45 ml) and acetone (5 ml). 1.63 g (62%) of a white powder is obtained. Melting point: 188-189° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06335445B1 |
| Source dataset | uspto-grants-2002_01 |
| ORD ID | ord-bedbdd7074744582a3744e2924caf1d1 |
| Source note | uspto-grants-2002_01 |