Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 2,6-Dimethylphenol | HCID 11335 | — |
| Reactant | Praseodymium oxide | HCID 165911 | — |
| Reactant | Alumina | HCID 9989226 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | HCID 178418361 | HCID 178418361 | — |
| Product | 2,6-Dimethylcyclohexylamine | HCID 110932 | 99.5% |
Reaction Steps
1.650 kg of 2,6-dimethylphenol and 150 g of a pulverulent catalyst which contains 5.0% by weight of palladium and 2.5% by weight of praseodymium oxide, the remainder being aluminum oxide, are introduced into a 10 l stirred autoclave. The autoclave is closed and 1.370 kg of ammonia are forced in. The mixture is then heated to 230° C. and a pressure of 200 bar is established by forcing in hydrogen. The mixture is kept at the reaction temperature until a constant pressure is achieved (about 8 hours). It is then left to cool, and is filtered to give 1.710 kg of crude 2,6-dimethylcyclohexylamine (a mixture of 3 stereoisomeric 2,6-dimethylcyclohexylamines). The crude product is distilled to give 1.685 kg of 2,6-dimethylcyclohexylamine, boiling point=167°-168° C., corresponding to a yield of 98%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04429155 |
|---|
| Source dataset | uspto-grants-1984_01 |
|---|
| ORD ID | ord-88a026750b744c7c9ed03bcef7aacd3f |
|---|
| Source note | uspto-grants-1984_01 |
|---|