反应详情

A solution of 2,3,4,4a-tetrahydro-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one 6.1 g. (0.03 mole) and 4.92 g. (0.03 mole) of 4-picolyl chloride hydrochloride, 10 g. of potassium carbonate, 0.5 ml. of tirethylamine in 200 ml. of acetone was refluxed for 40 hours with stirring. The reaction mixture was allowed to cool and the precipitate was filtered and washed with acetone. The acetone was removed under reduced pressure and the oily residue was dissolved in methylene chloride. This solution was washed with water, dried over magnesium sulfate, filtered and the solvent removed. The residue was dissolved in ethanol and treated with dry hydrogen chloride. The product hydrogen chloride was filtered and recrystallized from methanol to give 2 g. of the title compound as the dihydrochloride salt, m.p. 253°-255° C.

1. temperatureto cool
2. filtrationthe precipitate was filtered
3. washwashed with acetone
4. customThe acetone was removed under reduced pressure
5. dissolutionthe oily residue was dissolved in methylene chloride
6. washThis solution was washed with water
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. customthe solvent removed
10. dissolutionThe residue was dissolved in ethanol
11. additiontreated with dry hydrogen chloride
12. filtrationThe product hydrogen chloride was filtered
13. customrecrystallized from methanol
14. customto give 2 g