HRID2235573
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of 2.00 g (9.70 mmol) of methyl 1-methyl-2-oxo-1,3-dihydro-2H-benzimidazole-7-carboxylate in 20 mL of phosphorous oxychloride was heated at 100° C. for 6 h. The reaction was concentrated in vacuo and the thus obtained residue was quenched with water and extracted with ethyl acetate. The organics were dried over sodium sulfate, filtered, and concentrated in vacuo. The thus obtained residue was purified via flash chromatography eluting with a solution of 20% ethyl acetate/hexanes to give 1.77 g (81%) of the title compound as white solids.
WORKUP
后处理
- concentrationThe reaction was concentrated in vacuo
- customthe thus obtained residue was quenched with water
- extractionextracted with ethyl acetate
- dry with materialThe organics were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe thus obtained residue was purified via flash chromatography
- washeluting with a solution of 20% ethyl acetate/hexanes