HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → (-)-cis-1,2-Dimethoxy-4-(2-aminocyclohexyl)benzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | (+/-)-cis1,2-Dimethoxy-4-(2-nitrocyclohexyl)benzene | HCID 15389590 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | (-)-cis-1,2-Dimethoxy-4-(2-aminocyclohexyl)benzene | HCID 14321190 | 88.4% |
Reaction Steps
125 g of (+/−)-cis-1,2-dimethoxy-4-(2-nitrocyclohexyl)benzene and 120 g of zinc powder or granules are suspended in 1300 ml of ethanol. 220 ml of acetic acid are added dropwise at boiling heat. The precipitate is filtered off with suction and washed with ethanol, and the filtrate is concentrated under reduced pressure. The residue is taken up in hydrochloric acid and extracted with toluene. The aqueous phase is rendered alkaline using 50% strength sodium hydroxide solution, the precipitate is filtered off with suction and the filtrate is extracted with toluene. The organic phase is dried using sodium sulfate and concentrated. 98 g of the title compound are obtained as a crystallizing oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06630483B2 |
| Source dataset | uspto-grants-2003_10 |
| ORD ID | ord-e98f641cd04f420ba9d0a504b52f791d |
| Source note | uspto-grants-2003_10 |