HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → (+)-Epibatidine dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | (-)-Epibatidine-L-tartrate | HCID 1204 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | (+)-Epibatidine dihydrochloride | HCID 21946437 | 36% |
Reaction Steps
Racemic-epibatidine 19 (42 mg, 0.2 mmol) was mixed with 77 mg (0.7 mmol) freshly prepared ethyl formamidinate hydrochloride and 129 mg (1.0 mmol) diisopropyl ethylamine in 1 ml acetonitrile. After stirring at room temperature for 48 hours, the mixture was acidified with 1.0M hydrogen chloride in ether. After evaporation in vacuo, the residue was separated on silica gel preparative thin layer chromatography, using a solvent system of 25% methanol in chloroform, to give 25 mg of the compound 45 as a hygroscopic solid. Yield 36%. MS(CI), 236, 238 (free base M+1). H1 -NMR (CD3OD). δ 3.40 (M, 1H, H2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06060473 |
| Source dataset | uspto-grants-2000_05 |
| ORD ID | ord-4d6ec82eb31a4bf2ba1c15fd54bc8be9 |
| Source note | uspto-grants-2000_05 |