反应详情

3-Methyl-4-nitrobenzyl bromide (1.00 g), 3,5-dimethylpiperidine (0.60 ml) and potassium carbonate (0.90 g) were dissolved in acetone (20 ml), followed by heating under reflux for 6 hours. The reaction solution was concentrated under reduced pressure, dissolved in chloroform (10 ml), poured into water (100 ml) and extracted with chloroform (50 ml). The organic layer was washed with saturated brine (100 ml), dried over anhydrous sodium sulfate and, after filtration, concentrated under reduced pressure. The residue was purified by silica gel flash column chromatography (developing solvent: n-hexane/ethyl acetate=10:1) to obtain the subject compound (NCR-7) (0.70 g, yield 61%) as a yellow oil.

1. temperatureby heating
2. temperatureunder reflux for 6 hours
3. concentrationThe reaction solution was concentrated under reduced pressure
4. dissolutiondissolved in chloroform (10 ml)
5. additionpoured into water (100 ml)
6. extractionextracted with chloroform (50 ml)
7. washThe organic layer was washed with saturated brine (100 ml)
8. dry with materialdried over anhydrous sodium sulfate
9. filtrationafter filtration
10. concentrationconcentrated under reduced pressure
11. customThe residue was purified by silica gel flash column chromatography (developing solvent: n-hexane/ethyl acetate=10:1)
12. customto obtain the subject compound (NCR-7) (0.70 g, yield 61%) as a yellow oil