反应详情

温度

40 °C

Dissolve methyl-(1-methyl-piperidin-4-yl)-(5-nitro-benzooxazol-2-yl)-amine (0.583 g, 2.01 mmol), in acetic acid (8 mL), and add iron (1.12 g, 20.1 mmol) to the solution. Stir the mixture at 40° C. for 3 h. Filter the reaction mixture through Celite® and wash with water/MeOH. Concentrate the reaction mixture in vacuo. Subject the residue to silica gel flash column chromatography, eluting with 10% 2N NH3 in MeOH/CH2Cl2, to yield the desired product (0.474 g, 91%). MS (ES+) 261.2 (M+1)+.

1. filtrationFilter the reaction mixture through Celite®
2. washwash with water/MeOH
3. concentrationConcentrate the reaction mixture in vacuo
4. washeluting with 10% 2N NH3 in MeOH/CH2Cl2