反应详情

In acetic acid (100 ml) was dissolved N-(1,3-dimethoxypropan-2-yl)-N-methyl-4-nitrobenzylamine (3.1 g), and to the mixture was added reduced iron (3.2 g) little by little. The mixture was stirred at room temperature overnight, and the solvent was evaporated. To the residue was added ethyl acetate, and precipitates were filtered off. The filtrate was washed with sodium hydroxide solution, water and saturated brine, and dried with anhydrous magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue dissolved in ethyl acetate. To the mixture was added 4N hydrochloric acid-ethyl acetate, and precipitates were filtered and washed with diethylether. The mixture was dissolved in water, and the mixture was neutralized with 1N sodium hydroxide solution and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and dried with anhydrous magnesium sulfate. Under reduced pressure, the solvent was evaporated to give 4-((N-(1,3-dimethoxypropan-2-yl)-N-methylamino)methyl)aniline (2.4 g) as red oil.

1. customthe solvent was evaporated
2. additionTo the residue was added ethyl acetate
3. customprecipitates
4. filtrationwere filtered off
5. washThe filtrate was washed with sodium hydroxide solution, water and saturated brine
6. dry with materialdried with anhydrous magnesium sulfate
7. customUnder reduced pressure, the solvent was evaporated
8. dissolutionthe residue dissolved in ethyl acetate
9. additionTo the mixture was added 4N hydrochloric acid-ethyl acetate
10. customprecipitates
11. filtrationwere filtered
12. washwashed with diethylether
13. dissolutionThe mixture was dissolved in water
14. extractionextracted with ethyl acetate
15. washThe organic layer was washed with water and saturated brine
16. dry with materialdried with anhydrous magnesium sulfate
17. customUnder reduced pressure, the solvent was evaporated