Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-(4-Chlorobutyl)pyridine | HCID 10953941 | — |
| Reactant | HCID 20339413 | HCID 20339413 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 20339421 | HCID 20339421 | — |
Reaction Steps
A solution of 4.2 g. (0.02 mole) of 8-fluoro-2,3,4,4a-tetrahydro-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, 7 g. (0.04 mole) of 4-(4-pyridyl)-1-chlorobutane, 8 g. of potassium carbonate, 5 g. of potassium iodide, and 0.5 ml. of triethylamine was stirred and refluxed in 200 ml. of acetone for 72 hours, cooled and filtered. The solvent was removed and the residue was dissolved in methylene chloride. This solution was washed with water and brine, dried over magnesium sulfate and filtered. The solvent was removed and the residue was chromatographed on 500 g. of Silicar, CC-7. Fractions eluted with 10% methanol in ethyl acetate afforded the product as a free base. This free base was dissolved in ethanol and treated with dry hydrogen chloride saturated ether. The product hydrochloride was filtered and recrystallized from methanol to give 2.3 g. of the title compound as the dihydrochloride salt, m.p. 262°-264° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04203987 |
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| Source dataset | uspto-grants-1980_05 |
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| ORD ID | ord-2fda4a9d47d64f8c95e0159097877108 |
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| Source note | uspto-grants-1980_05 |
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