反应详情

A mixture of 7.1 g. of 2,3,4,4a-tetrahydro-3-methyl- 1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, 3.5 g. of lithium aluminum hydride and 450 ml. of dry tetrahydrofuran is refluxed for 20 hours under a nitrogen atmosphere. The mixture is cooled and 20 ml. of concentrated ammonium hydroxide is carefully added. The mixture is filtered and the filter cake is washed with isopropanol. The filtrate is concentrated to give 5.7 g. of product as a viscous oil. A 3.5 g. portion is dissolved in acetone and treated with a saturated solution of fumaric acid in acetone. Filtration gives 3.3 g. of the product as the fumaric acid salt, m.p. 178°-188°. Recrystallization from isopropanol gives 2.1 g. of salt, m.p. 186°-188° .

1. additionA mixture of 7.1 g
2. temperatureThe mixture is cooled
3. filtrationThe mixture is filtered
4. washthe filter cake is washed with isopropanol
5. concentrationThe filtrate is concentrated
6. customto give 5.7 g
7. filtrationFiltration
8. customgives 3.3 g
9. customRecrystallization from isopropanol
10. customgives 2.1 g