反应详情

温度

100 °C

Dissolve 2-ethylsulfanyl-5-nitro-benzooxazole (1.17 g, 5.23 mmol) in anhydrous THF (10 mL) in a reaction tube and blow nitrogen into the vessel for 10 s. Add methyl-(1-methyl-piperidin-4-yl)-amine (1.37 mL, 9.42 mmol) to the solution. Quickly seal the vessel and immerse into a pre-heated oil bath (100° C.) and stir for 24 h. Concentrate the reaction mixture in vacuo, wash with 1.0M NaOH (aq) (2×50 mL), dry over Na2SO4, filter, and concentrate in vacuo. Subject the residue by silica gel flash column chromatography, eluting with 2N NH3 in MeOH/CH2Cl2, to yield the desired product (0.608 g, 40%). MS (ES+) 291.0 (M+1)+.

1. customfor 10 s
2. customQuickly seal the vessel
3. customimmerse into a pre-heated oil bath
4. concentrationConcentrate the reaction mixture in vacuo
5. washwash with 1.0M NaOH (aq) (2×50 mL)
6. dry with materialdry over Na2SO4
7. filtrationfilter
8. concentrationconcentrate in vacuo
9. washeluting with 2N NH3 in MeOH/CH2Cl2