反应详情

A solution of 6 g. (0.03 mole) of 2,3,4,4a-tetrahydro-6-methyl-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, 5 g. (0.03 mole) of 4-picolyl chloride hydrochloride, 10 g. of potassium carbonate and 0.5 ml. of triethylamine was stirred and refluxed in 200 ml. of acetone overnight, 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 460 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 yield 5.2 g. of the title compound as the dihydrochloride salt, m.p. 252°-254.5° C.

1. temperaturerefluxed in 200 ml
2. filtrationfiltered
3. customThe solvent was removed
4. dissolutionthe residue was dissolved in methylene chloride
5. washThis solution was washed with water and brine
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. customThe solvent was removed
9. customthe residue was chromatographed on 460 g
10. washFractions eluted with 10% methanol in ethyl acetate
11. customafforded the product as a free base
12. filtrationThe product hydrochloride was filtered
13. customrecrystallized from methanol
14. customto yield 5.2 g