HRID410215
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
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).
WORKUP
后处理
- temperatureto reflux
- customUpon completion, POCL3 was evaporated off
- additionThe reaction mixture was diluted with water and saturated sodium bicarbonate
- extractionextracted with DCM
- extractionThe organic extract
- washwas washed with sat. sodium bicarbonate solution, water, brine
- dry with materialdried with, magnesium sulfate
- filtrationfiltered
- concentrationconcentrated