HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 21200669, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | 4-Hydroxy-3,3,5-trimethylcyclohexanone | HCID 21200670 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 21200669 | HCID 21200669 | — |
Reaction Steps
156 g of 3,3,5-trimethyl-4-hydroxycyclohexanon (formula VIa), 12 g of ammonium acetate and 60 g of Raney Ni in 250 ml methanol were hydrogenated at 100° C. under a hydrogen pressure of 100 bar in the presence of 250 ml of ammonia. When the uptake of hydrogen was complete, the catalyst was filtered off, the filtrate was concentrated under vacuum and the residue was subjected to fractional distillation under a high vacuum. 130 g of the aminoalcohol of formula Ic, which had a melting point of 110 to 112° C., were obtained at 90 to 97° C. (0.1 mbar). According to analysis by gas chromatography, an isomer mixture (four isomers) was present.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06242641B1 |
| Source dataset | uspto-grants-2001_06 |
| ORD ID | ord-95463e942bad43e6a61808a51dd2f6b4 |
| Source note | uspto-grants-2001_06 |