反应详情

A solution of 6.2 g. (0.03 mole) of 2,3,4,4a-tetrahydro-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, hydrochloride, 7 g. (0.04 mole) of 4-(4-pyridyl)-1-chlorobutane, 10 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 48 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 3.2 g. of free base. 3 G. of the above 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 3.2 g. of the title compound as the dihydrochloride salt, m.p. 281°-283° C.

1. temperaturerefluxed in 200 ml
2. temperaturecooled
3. filtrationfiltered
4. customThe solvent was removed
5. dissolutionthe residue was dissolved in methylene chloride
6. washThis solution was washed with water and brine
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. customThe solvent was removed
10. customthe residue was chromatographed on 500 g
11. washFractions eluted with 10% methanol in ethyl acetate
12. customafforded 3.2 g
13. filtrationThe product hydrochloride was filtered
14. customrecrystallized from methanol
15. customto give 3.2 g