HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formic Acid → 2-(beta-Methoxyethyl)amino-6-(beta-methoxyethyl)aminonitrobenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Methane | HCID 297 | — |
| Reactant | 4-Chloro-2-(beta-methoxyethyl)amino-6-(beta-methoxyethyl)aminonitrobenzene | HCID 20071082 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | 2-(beta-Methoxyethyl)amino-6-(beta-methoxyethyl)aminonitrobenzene | HCID 20071069 | — |
Reaction Steps
0.4 g of palladium at a concentration of 10% on active charcoal is added to 0.084 mole (25.5 g) of 4-chloro-2-(β-methoxyethyl)amino-6-(β-methoxyethyl)aminonitrobenzene in 33.4 ml of triethylamine, after which 7 ml of formic acid are added dropwise. At the end of the additions, the reaction mixture is heated for 1 hour 30 minutes, under reflux. The reaction mixture is diluted with 100 ml of 96° alcohol and 100 ml of water. The expected product precipitates. After filtration, the expected product containing the catalyst is dissolved in 90 ml of isopropyl alcohol. The catalyst is removed by hot filtration. The expected product crystallizes.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04992586 |
| Source dataset | uspto-grants-1991_02 |
| ORD ID | ord-abb8d79a029b42918187e3d6971550f6 |
| Source note | uspto-grants-1991_02 |