HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → (+/-)-cis-6-(3,4-Dimethoxyphenyl)-cyclohex-3-enylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | (+/-)-cis-1 2-Dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene | HCID 15389588 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | (+/-)-cis-6-(3,4-Dimethoxyphenyl)-cyclohex-3-enylamine | HCID 86601281 | 32.4% |
Reaction Steps
40 g of (±)-cis-1,2-dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene (compound F7) are dissolved in 400 ml of ethanol and 40 g of zinc powder are added. After heating to boiling temperature, 65 ml of glacial acetic acid are added dropwise. Afterwards, the reaction mixture is filtrated and concentrated. The residue is redissolved in diluted hydrochloric acid and extracted with toluene. The aqueous layer is alkalized using 6 N solution of sodium hydroxide and extracted several times with toluene. The combined organic phases of the alkalic extraction are dried using sodium sulfate and concentrated. The residue is chromatographed on silica gel. 11.5 g of the title compound are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08883818B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-c142d8147a4b46bea6095ba7276dd21c |
| Source note | uspto-grants-2014_11 |