反应详情

To a round bottomed flask was added 4-methoxy-1H-benzo[d]imidazol-2(3H)-one (1.8163 g, 11.06 mmol). POCl3 (1.031 mL, 11.06 mmol) was added and the reaction was brought to reflux. Upon completion, POCL3 was evaporated off. The residue was taken up in DCM. The reaction mixture was diluted with water and saturated sodium bicarbonate and extracted with DCM. The organic extract was washed with sat. sodium bicarbonate solution, water, brine, dried with magnesium sulfate, filtered, and concentrated to provide 2-Chloro-7-methoxy-1H-benzo[d]imidazole. MS (ESI, pos. ion) m/z: 182.9 (M+1).

1. temperatureto reflux
2. customUpon completion, POCL3 was evaporated off
3. additionThe reaction mixture was diluted with water and saturated sodium bicarbonate
4. extractionextracted with DCM
5. extractionThe organic extract
6. washwas washed with sat. sodium bicarbonate solution, water, brine
7. dry with materialdried with magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated