反应详情

温度

0 °C

To a solution of 4-p-tolyloxy-phenylamine (0.87 g, 4.38 mmol) and pyridine (0.52 mL, 6.53 mmol) in dried CH2Cl2 (10 mL) under N2 at 0° C. was added methanesulfonyl chloride (0.41 mL, 5.26 mmol) dropwise. The mixture was stirred at 0° C. for 1 h and was then poured into CH2Cl2/H2O (10 mL/10 mL). The organic layer was washed with 2N HCl (aq) (3 mL), H2O, brine, dried (Na2SO4), and filtered through Celite. After removal of solvent, the crude product was purified by chromatography (silica gel, 45% EtOAc/hexanes) to give the titled compound. MS (EI) 278 (M+H)+.

1. washThe organic layer was washed with 2N HCl (aq) (3 mL), H2O, brine
2. dry with materialdried (Na2SO4)
3. filtrationfiltered through Celite
4. customAfter removal of solvent
5. customthe crude product was purified by chromatography (silica gel, 45% EtOAc/hexanes)